KR20140016220A - Coating layer with nano multi-layer, method and apparatus for forming the smae - Google Patents

Abstract

Disclosed are a nanomulti-layer coating layer, a method and an apparatus for forming the same. The method for forming a nanomulti-layer coating layer by using a physical vapor deposition system having a sputtering apparatus and an arc ion plating apparatus comprises: a first coating step for forming a Mo coating layer on a basic material by using Ar gas and a Mo target of the sputtering apparatus; a nitrating step for forming a nitride thin film formation atmosphere by using N2 gas and Ar gas of the arc ion plating apparatus; a second coating step for forming a nanocomplex coating layer of Cr-Mo-N on the basic material by using Ar gas and the Mo target of the sputtering apparatus, and a Cr source, N2 gas, and Ar gas of the arc ion plating apparatus at the same time; and a multi-coating step for coating the basic material with a multi-layer where the nanocomplex coating layer of Cr-Mo-N and the Mo coating layer are repeated by revolving the basic material around a rotation axis. [Reference numerals] (AA) Start; (BB) End; (S100) First coating step; (S200) Nitrating step; (S300) Second coating step; (S400) Multi-coating step

Description

Nano multilayer coating layer, method for forming and forming device {COATING LAYER WITH NANO MULTI-LAYER, METHOD AND APPARATUS FOR FORMING THE SMAE}

The present invention relates to a nano-layer coating layer, a method for forming the same and a forming apparatus for controlling the direction of crystal growth to improve corrosion resistance and electrical conductivity.

In general, plasma coating technology is to apply a third material to the workpiece by using a plasma phenomenon in a vacuum state to add mechanical and functional properties that the original base material does not have, usually chemical vapor deposition (CVD) ) And physical vapor deposition (PVD).

As physical vapor deposition, vacuum deposition, sputtering, ion plating, and the like are widely used. Of these, ion plating is dependent on plasma activation and coating material ionization. It is named after various types of coating methods.

The arc ion plating method is to evaporate and ionize a target by using an arc discharge using a coating material (target) as a cathode. The coating speed is fast due to a rapid evaporation rate, and thus the productivity is high, and has high ionization, collision, and moving energy. It has been usefully used for hard coatings.

However, coating materials having excellent corrosion resistance generally have a problem of poor conductivity. For example, CrN has excellent corrosion and abrasion resistance but low electrical conductivity. Conventionally, the Cr ₂ N phase was formed on the CrN coating layer to improve the electrical conductivity, which was used as a surface coating material for parts such as fuel cell separators requiring corrosion resistance and electrical conductivity, but the electrical conductivity characteristics were somewhat insufficient.

An object of the present invention is to improve the corrosion resistance and electrical conductivity by using a functional metal having excellent conductivity in the CrN coating layer for the microstructure and the multilayer layer and controlling the direction of crystal growth through controlling the bias voltage during the coating process.

It should be understood that the foregoing description of the background art is merely for the purpose of promoting an understanding of the background of the present invention and is not to be construed as an admission that the prior art is known to those skilled in the art.

JP 2004-323883 A

The present invention has been proposed to solve the above problems, and an object of the present invention is to provide a nano-layer coating layer, a method for forming the same, and a device for improving the corrosion resistance and electrical conductivity by controlling the direction of crystal growth.

Nano-layer coating layer forming method according to the present invention for achieving the above object, as a coating layer forming method using a sputtering mechanism and an arc ion plating mechanism, the Mo coating layer using the Mo target and Ar gas of the sputtering mechanism to the base material Forming a first coating step; A nitriding step of forming a nitride thin film forming atmosphere using Ar gas and N ₂ gas of the arc ion plating apparatus; A second coating step of forming a nano-composite coating layer of Cr-Mo-N on the base material by using the Mo target of the sputtering mechanism and the Ar gas of the sputtering mechanism and the Ar gas, the N ₂ gas, and the Cr source simultaneously; And coated with a multi-layer repeating nano-composite coating layer and Mo coating layer of Cr-Mo-N on the base material, by applying a bias voltage of -250 ~ -150V to the base material to include the main growth surface of Cr-Mo-N [220] It includes; multi-coating step to be.

In the multi-coating step, the sputtering mechanism and the arc ion plating mechanism may maintain an angle between 60 and 120 degrees between central axes.

The multi-coating step may control the Ar gas of the sputtering mechanism at a flow rate of 60 sccm, the Ar gas of the arc ion plating mechanism is controlled at 20 sccm, and the N ₂ gas may be controlled at a flow rate of 40 to 100 sccm.

The multi-coating step may control the power of the sputtering mechanism to 50 ~ 1000 W.

The multi-coating step may maintain the temperature in the chamber at 150 ~ 350 ℃.

In the multi-coating step, [111], [200] and [220] may be included in the main growth surface of Cr-Mo-N.

Nano-layer coating layer forming apparatus of the present invention, the chamber is provided so that the base material can rotate; A sputtering mechanism for providing a Mo target and an Ar gas in a predetermined range in the chamber; An arc ion plating mechanism for providing an Ar gas, an N ₂ gas, and a Cr source in a predetermined range in the chamber; And controlling the Mo target and the Ar gas of the sputtering mechanism to form a Mo coating layer on the base material, and controlling the Ar gas and the N ₂ gas of the arc ion plating mechanism to form a nitride thin film forming atmosphere, and the Mo target of the sputtering mechanism. And control the Ar gas, N ₂ gas and Cr source of the Ar gas and arc ion plating apparatus at the same time to form a nano-composite coating layer of Cr-Mo-N on the base material, and nano-composite coating layer of Cr-Mo-N on the base material And a Mo coating layer to be repeatedly formed, the control unit to be included in the main growth surface of the Cr-Mo-N by the bias voltage applied to the base material -250 ~ -150V.

The coating layer prepared by the method for forming the nano-layer coating layer, Cr-Mo-N nano-composite coating layer and Mo coating layer is repeatedly laminated with a nano multi-layer, the bias voltage of the base material is controlled by -250 ~ -150V Cr [220] may be included in the main growth plane of -Mo-N.

In addition, the main growth surfaces of Cr-Mo-N may be [111], [200], and [220].

According to the nano multi-layer coating layer, the formation method and the forming device having the structure as described above, in the surface treatment for fuel cell separator plate through a significant improvement in electrical conductivity through functional metal nanocomposite and control of the microstructure of the existing CrN coating layer It is possible to improve the electrical conductivity and thus the weldability of the parts used and coating material applied.

In addition, as compared with the existing CrN coating layer, not only corrosion resistance but also electric conductivity is secured and hardness is improved.

1 is a flow chart of the nano-layer coating layer forming method according to an embodiment of the present invention.
Figure 2 is a block diagram of a nano-layer coating layer forming apparatus according to an embodiment of the present invention.
Figure 3 is a microstructure photograph of the nano-layer coating layer according to an embodiment of the present invention.
Figure 4 is a graph showing the phase change according to the bias voltage of the nano-layer coating layer according to an embodiment of the present invention.
5 to 7 is a graph showing the effect of the nano-layer coating layer according to an embodiment of the present invention.

Hereinafter, with reference to the accompanying drawings looks at with respect to the nano-layer coating layer according to a preferred embodiment of the present invention, a method of forming and forming apparatus.

1 is a flow chart of a method for forming a nano-layer coating layer according to an embodiment of the present invention, the method for forming a nano-layer coating layer of the present invention, a method for forming a coating layer using a sputtering mechanism and an arc ion plating mechanism, sputtering on the base material A first coating step S100 of forming a Mo coating layer using an Mo target and an Ar gas of the apparatus; Nitriding step (S200) to form a nitride film forming atmosphere using the Ar gas and N ₂ gas of the arc ion plating mechanism; A second coating step (S300) of forming a nano-composite coating layer of Cr-Mo-N by simultaneously using a Mo target of the sputtering mechanism, an Ar gas, and an Ar gas, an N ₂ gas, and a Cr source of the sputtering mechanism; And a multi-coating step (S400) of coating the base material with a multi-layer in which the nano-composite coating layer of Cr-Mo-N and the Mo coating layer are repeated by revolving around the rotation axis.

The method for forming a nano-layer coating layer of the present invention basically uses a physical vapor deposition machine, and uses a sputtering device 100 and an arc ion plating device 300.

2 is a configuration diagram of a nano-layer coating layer forming apparatus according to an embodiment of the present invention, the base material (M) inside the chamber (C) is provided to rotate and rotate at the same time based on the rotating shaft (H) in the interior do. And the sputtering mechanism 100 and the arc ion plating mechanism 300 are spaced apart from the side of the base material (M). The sputtering mechanism 100 provides Mo target and Ar gas in a range within the chamber C, and the arc ion plating mechanism 300 supplies Ar gas, N ₂ gas, and Cr source in the chamber C. Provided in a certain range.

Through this, the base material (M) is coated by the influence of the sputtering mechanism (100) while being idle or is simultaneously affected by the sputtering mechanism (100) and the arc plating mechanism (300). In addition, the base material (M) is installed to rotate at the same time to be evenly coated on the front. Such a device is also referred to as a "hybrid type physical vapor deposition machine," such a device is a device for forming a nano-layer coating layer of the present invention will be described below.

Specifically, the present invention is to form a nano-composite and nano multi-layer using a functional metal (Mo), forming a nano-composite coating (Cr-Mo-N) and Cr-Mo-N using Mo / Mo nanolayer structure can be formed by depositing each element using two ion sources, and controlling the source power, deposition time and jig rotation / revolution speed. Then, by controlling the crystallization direction by adjusting the bias voltage it can be controlled to include [220] in the main growth surface of the Cr-Mo-N.

First, in order to implement the present invention, a hybrid physical vapor deposition machine equipped with asymmetric magnetron sputtering and arc ion plating (AIP), respectively, was used as an apparatus for coating.

And the base material for deposition is fixed using a jig within the effective height (120mm) section of each sputtering target 120 and the ion plating target 320, the distance from each target is adjusted to within 80 ~ 150mm to adjust the deposition process The base material position was fixed.

The vacuum level of the preparation step for deposition was 2 * 10 ^ -2 torr, and the vacuum level was adjusted until 4 * 10 ^ -5 torr.

Thereafter, the base fixing jig was revolved at a speed of within 2 to 10 RPM during the deposition process to form an intermediate multilayer film having a uniform film structure and a nanoscale single metal composition.

First, before forming the multi-component functional layer, a metal (Mo) buffer layer for increasing adhesion with a sample is formed. That is, a first coating step (S100) is performed to form a Mo coating layer using an Mo target and an Ar gas of the sputtering mechanism on the base material. To this end, sputtering deposition is performed using an Mo target in an Ar (1-100 sccm, sputtering region) atmosphere.

In addition, a nitriding step (S200) is performed to form a nitride thin film forming atmosphere using Ar gas and N ₂ gas of the arc ion plating apparatus. To this end, the amount of Ar gas to be sputtered is reduced, the Ar gas to the ion-plating side is added, and the N ₂ gas is added to provide an atmosphere for forming a multi-component nitride thin film.

And a second coating step (S300) of forming a nano-composite coating layer of Cr-Mo-N by simultaneously using a Mo target of an sputtering mechanism, an Ar gas, and an Ar gas, an N ₂ gas, and a Cr source on a base material. And by performing a multi-coating step (S400) to coat the base material by the revolving axis around the nano-composite coating layer of Cr-Mo-N and a multi-coating layer repeated Mo. For this purpose, Cr-Mo-N multicomponent nanocomposite coating is formed by simultaneously using the source of sputtering device (Mo) and arc ion plating device (Cr) while maintaining the deposition vacuum at 8 * 10 ^ -3 torr. will be.

On the other hand, the multi-coating step (S400) is the sputtering mechanism and the arc ion plating mechanism to maintain the angle between the center axis between the 60 to 120 degrees. Because, when the rotation of the base material (M) is located at an angle outside the common source supply range of the sputtering device 100 and the arc ion plating device 300, only nanocomposite grains are formed and a multilayer made of functional metal This is because the film cannot be formed.

That is, the sputtering mechanism 100 and the arc ion plating mechanism 300 maintain the Cr-Mo-N multicomponent nanocomposite coating layer in an overlapping source supply section by maintaining an angle between 60 and 120 degrees between central axes. It is. In the case of the Mo coating layer, the coating is made in an area included only in the source supply range of the sputtering apparatus 100. As a result, the Mo coating layer and the Cr-Mo-N coating layer each have one revolution while the base material M rotates. It is formed by one layer.

In addition, when N ₂ is introduced into the source side of the sputtering apparatus 100 or N ₂ gas is entirely injected into the chamber, the N ₂ gas is necessarily an arc ion plating mechanism 300 because a multilayer film made of a functional metal cannot be formed. Supply only to the side.

In addition, the multi-coating step (S400) may be such that the bias voltage applied to the base material (M) is -250 ~ -150V. This is because when the bias voltage of -250 ~ -150V is applied to the base material (M), it is included in the main growth surface of Cr-Mo-N can be provided with both conductivity and hardness and corrosion resistance.

4 is a graph showing a phase change according to a bias voltage of a nano-layer coating layer according to an embodiment of the present invention. In the case of a bias voltage of -80V, the main growth surface is [111], [200] or -200V. In the case of applying a voltage, [220] is included in the main growth surface, and it can be seen that the conductivity and corrosion resistance are excellent in the bias voltage range of -250 to -150V.

More specifically, as shown in FIG. 5, the main growth surface of Cr-Mo-N is represented by [220] from the bias voltage of -140V. In the case of the bias voltage of −500 V or less, the main growth surface is not observed. Therefore, the bias voltage should not exceed -150V. Figure 6 is a graph of the conductivity evaluation accordingly, it can be seen that the resistance is reduced from the bias voltage -140V, the lowest at -200V. Therefore, the bias voltage should not exceed -150V, because [220] is included in the main growth surface of Cr-Mo-N.

On the other hand, in Fig. 5 it can be seen that the main growth surface [111] of Cr-Mo-N is not observed when the bias voltage is -300V. In addition, in view of FIG. 7, which is a result of the hardness evaluation, the hardness of the steel is significantly lowered from -300 V to 25 GPa with the phenomenon that the main growth surface [111] of Cr-Mo-N is not observed when the bias voltage is -300 V. As a result, it can be seen that it is difficult to use as a vehicle component. Thus, it can be seen that at least the bias voltage must exceed -250V, which is between -200V and -300V.

Therefore, as supported by these test results, the bias voltage applied to the base material in the multi-coating step is effective by having the main growth surface that is most needed in terms of electrical conductivity, durability and hardness. will be.

On the other hand, the multi-coating step (S400) controls the Ar gas of the sputtering mechanism at a flow rate of 60 sccm, the Ar gas of the arc ion plating mechanism is controlled at 20 sccm, and the N ₂ gas is controlled at a flow rate of 40-100 sccm Do it.

In addition, the multi-coating step (S400) to control the power of the sputtering mechanism to 50 ~ 1000W, to form the Mo coating layer and Cr-Mo-N coating layer alternately while maintaining the temperature in the chamber at 150 ~ 350 ℃ .

Figure 3 is a microstructure photograph of the nano-layer coating layer according to an embodiment of the present invention, the relatively thick Cr-Mo-N coating layer and the relatively thin Mo coating layer alternate through the multi-coating step (S400) It can be seen that the coating.

On the other hand, Figure 2 is a block diagram of a nano-layer coating layer forming apparatus according to an embodiment of the present invention, the nano-layer coating layer forming apparatus of the present invention, the base material (M) is rotated on the basis of the internal axis (H) A chamber (C) provided to revolve; A sputtering mechanism (100) for providing Mo target and Ar gas in a predetermined range in the chamber (C); An arc ion plating mechanism (300) for providing Ar gas, N ₂ gas, and Cr source in a predetermined range in the chamber (C); And controlling the Mo target and the Ar gas of the sputtering mechanism 100 so that the Mo coating layer is formed on the base material M, and controlling the Ar gas and the N ₂ gas of the arc ion plating mechanism 300 to form a nitride thin film formation atmosphere. And control the Mo target of the sputtering mechanism 100 and the Ar gas and the Ar gas, N ₂ gas and the Cr source of the arc ion plating mechanism 300 at the same time to control the nano-material of Cr-Mo-N in the base material (M) And a control unit 700 for forming a composite coating layer and revolving the base material M about the rotation axis H so that the nanocomposite coating layer of Cr-Mo-N and the Mo coating layer are repeatedly formed.

The temperature of the chamber C is controlled by the controller 700, and the inside of the chamber C is controlled by the controller 700 so that the base material M rotates and rotates. In addition, the Mo target 120 is installed in the sputtering mechanism 100, an Ar gas supply is provided, and a power supply unit 140 is provided. Meanwhile, the arc ion plating mechanism 300 is provided with a Cr source 320, an Ar gas and an N ₂ gas supplier, and a power providing unit 340. In the chamber C, a bias voltage generation unit 500 for supplying a bias voltage to the base material M is provided.

The control unit 700 controls the operation of the sputtering mechanism 100 and the arc ion plating mechanism 300.

The controller 700 controls the Mo target 120 and the Ar gas of the sputtering mechanism 100 so that the Mo coating layer is formed on the base material M, and the Ar gas and the N ₂ gas of the arc ion plating mechanism 300. To form a nitride thin film formation atmosphere, and simultaneously control the Mo target 120 and the Ar gas, the N ₂ gas and the Cr source 320 of the Ar gas and the arc ion plating mechanism 300 of the sputtering mechanism 100. To form a nano-composite coating layer of Cr-Mo-N on the base material (M), and revolve the base material (M) around the rotation axis (H) to form the nano-composite coating layer and Cr coating layer of Cr-Mo-N repeatedly. Be sure to This is to repeat the nano-composite coating layer and Mo coating layer of Cr-Mo-N as shown in FIG.

While the present invention has been particularly shown and described with reference to specific embodiments thereof, it will be understood by those skilled in the art that various changes in form and details may be made therein without departing from the spirit and scope of the invention as defined by the following claims It will be apparent to those of ordinary skill in the art.

100: sputtering mechanism 300: arc ion plating mechanism
500: bias voltage generation unit 700: control unit
C: Chamber M: Base Material

Claims (9)

As a method of forming a coating layer using a sputtering mechanism and an arc ion plating mechanism,
A first coating step (S100) of forming a Mo coating layer using a Mo target and an Ar gas of a sputtering mechanism on a base material;
Nitriding step (S200) to form a nitride film forming atmosphere using the Ar gas and N ₂ gas of the arc ion plating mechanism;
A second coating step (S300) of forming a nano-composite coating layer of Cr-Mo-N by simultaneously using a Mo target of the sputtering mechanism and an Ar gas of the sputtering mechanism and an Ar gas, an N ₂ gas, and a Cr source of the arc ion plating mechanism; And
The nanocomposite coating layer of the Cr-Mo-N and the Mo coating layer are coated on the base material with a repeating multilayer, and the main growth surface of the Cr-Mo-N is included by applying a bias voltage of -250 ~ -150V to the base material. Nano coating layer forming method comprising a; multi-coating step (S400). The method according to claim 1,
The multi-coating step (S400) is a method for forming a nano-layer coating layer, characterized in that the sputtering mechanism and the arc ion plating mechanism to maintain the angle between the center axis between 60 to 120 degrees. The method according to claim 1,
The multi-coating step (S400) to control the Ar gas of the sputtering mechanism to a flow rate of 60 sccm, to control the Ar gas of the arc ion plating mechanism to 20 sccm and to control the N ₂ gas at a flow rate of 40 ~ 100 sccm Nano-layer coating layer forming method characterized in that. The method according to claim 1,
The multi-coating step (S400) is a method for forming a nano-layer coating layer, characterized in that to control the power of the sputtering mechanism to 50 ~ 1000 W. The method according to claim 1,
The multi-coating step (S400) is a method for forming a nano-layer coating layer, characterized in that to maintain the temperature in the chamber at 150 ~ 350 ℃. The method according to claim 1,
In the multi-coating step (S400), [111], [200] and [220] are included in the main growth surface of Cr-Mo-N. A chamber C provided to rotate the base material M;
A sputtering mechanism (100) for providing Mo target and Ar gas in a predetermined range in the chamber (C);
An arc ion plating mechanism (300) for providing Ar gas, N ₂ gas, and Cr source in a predetermined range in the chamber (C); And
By controlling the Mo target and the Ar gas of the sputtering mechanism 100 to form a Mo coating layer on the base material (M), by controlling the Ar gas and N ₂ gas of the arc ion plating mechanism 300 to create a nitride thin film formation atmosphere The nano-composite of Cr-Mo-N in the base material M is formed by simultaneously controlling the Mo target of the sputtering device 100 and the Ar gas, the N ₂ gas, and the Cr source of the arc ion plating device 300. The coating layer is formed, and the nano-composite coating layer and the Mo coating layer of Cr-Mo-N are repeatedly formed on the base material (M), but the Cr-Mo by applying a bias voltage applied to the base material (M) to -250 ~ -150V. Nano-layer coating layer forming apparatus comprising a; control unit 700 to be included in the main growth surface of -N. As a coating layer prepared by the method for forming a nano-layer coating layer of claim 1,
Nano-composite coating layer and Mo-coating layer of Cr-Mo-N are repeatedly stacked with nano multi-layer, but the bias voltage of the base material is controlled to be -250 ~ -150V so that [220] is included in the main growth surface of Cr-Mo-N. Nano multilayer coating layer, characterized in that. The method according to claim 8,
Nano-layer coating layer characterized in that the main growth surface of the Cr-Mo-N [111], [200] and [220].

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