KR20050069940A - Deposition of super hard tialsin thin films by cathodic arc plasma deposition - Google Patents

Deposition of super hard tialsin thin films by cathodic arc plasma deposition Download PDF

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KR20050069940A
KR20050069940A KR1020050031701A KR20050031701A KR20050069940A KR 20050069940 A KR20050069940 A KR 20050069940A KR 1020050031701 A KR1020050031701 A KR 1020050031701A KR 20050031701 A KR20050031701 A KR 20050031701A KR 20050069940 A KR20050069940 A KR 20050069940A
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tialsin
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chamber
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KR100659743B1 (en
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김선규
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울산대학교 산학협력단
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    • CCHEMISTRY; METALLURGY
    • C23COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23CCOATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/22Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
    • C23C14/24Vacuum evaporation
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B23MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
    • B23PMETAL-WORKING NOT OTHERWISE PROVIDED FOR; COMBINED OPERATIONS; UNIVERSAL MACHINE TOOLS
    • B23P15/00Making specific metal objects by operations not covered by a single other subclass or a group in this subclass
    • B23P15/28Making specific metal objects by operations not covered by a single other subclass or a group in this subclass cutting tools
    • CCHEMISTRY; METALLURGY
    • C23COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23CCOATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/22Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
    • C23C14/34Sputtering
    • C23C14/3464Sputtering using more than one target
    • CCHEMISTRY; METALLURGY
    • C23COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23CCOATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/22Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
    • C23C14/34Sputtering
    • C23C14/35Sputtering by application of a magnetic field, e.g. magnetron sputtering
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01LSEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L21/00Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
    • H01L21/67Apparatus specially adapted for handling semiconductor or electric solid state devices during manufacture or treatment thereof; Apparatus specially adapted for handling wafers during manufacture or treatment of semiconductor or electric solid state devices or components ; Apparatus not specifically provided for elsewhere
    • H01L21/67005Apparatus not specifically provided for elsewhere
    • H01L21/67011Apparatus for manufacture or treatment
    • H01L21/67155Apparatus for manufacturing or treating in a plurality of work-stations
    • H01L21/67207Apparatus for manufacturing or treating in a plurality of work-stations comprising a chamber adapted to a particular process

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Abstract

본 발명은 음극아크증착을 이용한 초고경도 TiAlSiN 박막 증착방법에 관한 것으로, Ti 타겟과, AlSi 타겟을 아크소스에 설치하거나, TiAlSi 복합타겟을 아크소스에 설치하여 질소 가스를 주입하면서 아크방전을 유기하여 플라즈마를 형성하여 피처리물의 표면에 TiAlSiN 코팅층을 형성하도록 함으로써 초고경도의 절삭공구를 제조하는 음극아크증착을 이용한 초고경도 TiAlSiN 박막 증착방법을 제공함에 그 목적이 있다.The present invention relates to a method for depositing ultra-high hardness TiAlSiN thin film using cathode arc deposition. The Ti target and the AlSi target are installed in an arc source, or the TiAlSi composite target is installed in an arc source to inject an arc discharge while injecting nitrogen gas. It is an object of the present invention to provide an ultra-hard TiAlSiN thin film deposition method using a cathode arc deposition to produce a cutting tool of ultra-hardness by forming a plasma to form a TiAlSiN coating layer on the surface of the workpiece.

본 발명은 음극아크증착을 이용한 초고경도 TiAlSiN 박막 증착을 위한 음극아크 증착공정은 크게 Ti타겟과 AlSi 타겟 혹은 TiAlSi 타겟을 설치하는 타겟설치과정과; 상기 타겟들 및 피처리물이 설치된 챔버 내부의 진공도를 10-5∼10-7 Torr로 낮춰 상기 챔버 내부의 공기를 제거하는 과정과; 상기 챔버로 불활성 가스를 주입하여 상기 챔버 내부의 진공도를 10-1∼10-3 Torr로 세팅하여 피처리물 표면을 세정하는 플라즈마 클리닝 과정과; 질소를 챔버에 유입시킨 후 아크소스에 전류를 인가하여 플라즈마를 형성하고 바이어스 전압을 인가하여 TiAlSiN 층을 형성하는 과정으로 이루어진 것을 특징으로 한다.The present invention provides a cathode arc deposition process for depositing ultra-hard TiAlSiN thin films using cathode arc deposition, comprising: a target installation process for installing a Ti target and an AlSi target or a TiAlSi target; Removing air in the chamber by lowering the degree of vacuum in the chamber in which the targets and the workpiece are installed to 10 −5 to 10 −7 Torr; A plasma cleaning process of injecting an inert gas into the chamber to clean the surface of the workpiece by setting a vacuum degree within the chamber to 10 −1 to 10 −3 Torr; After nitrogen is introduced into the chamber, a current is applied to the arc source to form a plasma, and a process of forming a TiAlSiN layer by applying a bias voltage.

본 발명을 적용하면, Ti 타겟에 인가되는 코팅전위는 18V이며, 코팅전류는 45A이고, AlSi 타겟에 인가하는 코팅전위는 19V이고, 코팅전류는 35A가 되도록 하여 음극 아크증착을 실시한 결과, 초고경도의 코팅박막을 얻게 되었다는 잇점이 있다.According to the present invention, the coating potential applied to the Ti target is 18V, the coating current is 45A, the coating potential applied to the AlSi target is 19V, and the coating current is 35A. This has the advantage of obtaining a coated thin film.

Description

음극아크증착을 이용한 초고경도 티아이에이엘에스아이엔 박막 증착방법{DEPOSITION OF SUPER HARD TiAlSiN THIN FILMS BY CATHODIC ARC PLASMA DEPOSITION}Ultra-high hardness TAI SL thin film deposition method using cathode arc deposition {DEPOSITION OF SUPER HARD TiAlSiN THIN FILMS BY CATHODIC ARC PLASMA DEPOSITION}

본 발명은 음극아크증착을 이용한 초고경도 TiAlSiN 박막 증착방법에 관한 것으로, 보다 상세하게 Ti 타겟과, AlSi 타겟을 아크소스에 설치하거나, TiAlSi 복합타겟을 아크소스에 설치하여 질소 가스를 주입하면서 아크방전을 유기하여 플라즈마를 형성하여 피처리물의 표면에 TiAlSiN 코팅층을 형성하도록 함으로써 초고경도의 절삭공구를 제조하는 음극아크증착을 이용한 초고경도 TiAlSiN 박막 증착방법에 관한 것이다.The present invention relates to a method of depositing ultra-high hardness TiAlSiN thin film using cathode arc deposition. More specifically, a Ti target and an AlSi target are installed in an arc source, or a TiAlSi composite target is installed in an arc source to inject nitrogen gas into an arc discharge. The present invention relates to a super-hardness TiAlSiN thin film deposition method using a cathode arc deposition to produce a cutting tool of ultra-hardness by forming a plasma by forming a plasma to form a TiAlSiN coating layer on the surface of the workpiece.

주지된 바와 같이, 최근에는 산업체에서 각종 금속재질들이 합금 경화성, 내구성 등의 향상시키기 위해 각종 코팅법이 적용되어 재질 향상에 기여하고 있는 바, 그와 같은 금속재질을 절삭하기 위한 절삭공구도 역시 강도가 강화되어야만 하였다.As is well known, in recent years, various metal coating materials have been applied in the industry to improve alloy hardenability, durability, and the like, thereby contributing to the improvement of materials, and cutting tools for cutting such metal materials are also strong. Had to be strengthened.

따라서, 최근에는 고경도의 티타늄(Ti) 재질을 절삭공구에 적용하면서도, 그 경도를 더욱 우수하게 하기 위해 각종 코팅방법이 적용되고 있다. 그 중 하나가 마그네트론 스퍼터링방법이다. 즉, 마그네트론 스퍼터링법을 이용하여 TiAlN 피복경질층에 Cr을 첨가한 TiAlCrN 피복 경질층을 TiAlN 피복경질층과 교차하여 적층으로 절삭공구에 코팅하므로써 기존의 TiAlN코팅공구 보다 피복 경질층의 경도 및 산화개시온도를 증가시켜 건식 고속가공이 가능한 경질 피복층의 제조방법이 개시되어 있는 현재까지의 기술이었다.Therefore, in recent years, while applying a high hardness titanium (Ti) material to the cutting tool, various coating methods have been applied to further improve the hardness. One of them is the magnetron sputtering method. In other words, the TiAlCrN coated hard layer containing Cr added to the TiAlN coated hard layer using the magnetron sputtering method is laminated to the cutting tool by laminating it with the TiAlN coated hard layer to start the hardness and oxidation of the coated hard layer than the conventional TiAlN coated tool. It has been the technique to date which the manufacturing method of the hard coat layer which can dry dry high speed processing by increasing temperature is disclosed.

하지만, 이러한 TiAlN 피복경질층에 Cr을 첨가한 TiAlCrN 피복 경질층을 마그네트론 스퍼터링법을 통해 형성한 절삭공구의 경우에는 TiAlN 피복경질층만으로 이루어진 절삭공구에 비해 그 경도가 우수하기는 하나, 큰 차이가 없었으므로 그 효과면에서 많은 상승효과를 기대하기 어려웠다는 문제가 있었다. However, in the case of a cutting tool in which the TiAlCrN coating hard layer containing Cr is added to the TiAlN coating hard layer by magnetron sputtering, the hardness of the cutting tool is superior to that of the cutting tool comprising only the TiAlN coating hard layer, but there is a big difference. There was a problem that it was difficult to expect many synergies in terms of the effect.

본 발명은 상기한 종래 기술의 사정을 감안하여 이루어진 것으로, Ti 타겟과, AlSi 타겟을 아크소스에 설치하거나, TiAlSi 복합타겟을 아크소스에 설치하여 질소 가스를 주입하면서 아크방전을 유기하여 플라즈마를 형성하여 피처리물의 표면에 TiAlSiN 코팅층을 형성하도록 함으로써 초고경도의 절삭공구를 제조하는 음극아크증착을 이용한 초고경도 TiAlSiN 박막 증착방법을 제공함에 그 목적이 있다.SUMMARY OF THE INVENTION The present invention has been made in view of the above-described prior art, and a plasma is formed by incorporating an arc discharge while injecting nitrogen gas by installing a Ti target and an AlSi target in an arc source or a TiAlSi composite target in an arc source. By forming a TiAlSiN coating layer on the surface of the workpiece to provide an ultra-hard TiAlSiN thin film deposition method using a cathode arc deposition to produce a cutting tool of ultra-hardness.

상기한 목적을 달성하기 위해, 본 발명의 바람직한 실시예에 따르면 음극아크증착을 이용한 초고경도 TiAlSiN 박막 증착을 위한 음극아크 증착공정은 크게 Ti타겟과 AlSi 타겟 혹은 TiAlSi 타겟을 설치하는 타겟설치과정과; 상기 타겟들 및 피처리물이 설치된 챔버 내부의 진공도를 10-5∼10-7 Torr로 낮춰 상기 챔버 내부의 공기를 제거하는 과정과; 상기 챔버로 불활성 가스를 주입하여 상기 챔버 내부의 진공도를 10-1∼10-3 Torr로 세팅하여 피처리물 표면을 세정하는 플라즈마 클리닝 과정과; 질소를 챔버에 유입시킨 후 아크소스에 전류를 인가하여 플라즈마를 형성하고 바이어스 전압을 인가하여 TiAlSiN 층을 형성하는 과정으로 이루어진 것을 특징으로 하는 음극아크증착을 이용한 초고경도 TiAlSiN 박막 증착방법이 제공된다.In order to achieve the above object, according to a preferred embodiment of the present invention, the cathode arc deposition process for depositing ultra-hard TiAlSiN thin film using cathode arc deposition includes a target installation process for installing a Ti target and an AlSi target or a TiAlSi target; Removing air in the chamber by lowering the degree of vacuum in the chamber in which the targets and the workpiece are installed to 10 −5 to 10 −7 Torr; A plasma cleaning process of injecting an inert gas into the chamber to clean the surface of the workpiece by setting a vacuum degree within the chamber to 10 −1 to 10 −3 Torr; Provided is a method for depositing ultra-high hardness TiAlSiN thin film using cathode arc deposition, comprising introducing a nitrogen into a chamber, applying a current to an arc source to form a plasma, and applying a bias voltage to form a TiAlSiN layer.

바람직하게, 상기 플라즈마 클리닝 과정은 에칭전위는 310∼320V, 에칭전류는 0.6A가 되도록 하며, 약 10분간 클리닝을 위한 에칭이 수행되도록 하는 것을 특징으로 하는 음극아크증착을 이용한 초고경도 TiAlSiN 박막 증착방법이 제공된다.Preferably, in the plasma cleaning process, the etching potential is 310 to 320V, the etching current is 0.6A, and the ultra-hardness TiAlSiN thin film deposition method using cathode arc deposition, characterized in that the etching is performed for about 10 minutes. This is provided.

바람직하게, 상기 Ti 타겟에 공급되는 전위 및 전류는 14∼22V, 35∼55A 이며, AlSi 타겟에 공급되는 전위 및 전류는 15∼23V, 25∼55A 인 것을 특징으로 하는 음극아크증착을 이용한 초고경도 TiAlSiN 박막 증착방법이 제공된다.Preferably, the potential and current supplied to the Ti target are 14 to 22 V and 35 to 55 A, and the potential and current supplied to the AlSi target are 15 to 23 V and 25 to 55 A. A TiAlSiN thin film deposition method is provided.

바람직하게, 상기 Ti 타겟 및 AlSi 타겟의 피처리물에 대한 증착온도는 200∼450℃인 것을 특징으로 하는 음극아크증착을 이용한 초고경도 TiAlSiN 박막 증착방법이 제공된다.Preferably, the ultra-hardness TiAlSiN thin film deposition method using a cathode arc deposition is provided, the deposition temperature of the Ti target and the AlSi target to be treated is 200 ~ 450 ℃.

이하, 본 발명에 대해 도면을 참조하여 상세하게 설명한다.EMBODIMENT OF THE INVENTION Hereinafter, this invention is demonstrated in detail with reference to drawings.

도 1은 본 발명의 일실시예에 따른 음극아크증착을 이용한 초고경도 TiAlSiN 박막 증착을 행하기 위한 음극아크 증착장치의 구성을 개략적으로 도시한 모식도이며, 도 2는 본 발명의 일실시예에 따른 음극아크증착을 이용한 초고경도 TiAlSiN 박막 증착공정을 도시한 플로우챠트이다.1 is a schematic diagram showing the configuration of a cathode arc deposition apparatus for performing ultra-hardness TiAlSiN thin film deposition using a cathode arc deposition according to an embodiment of the present invention, Figure 2 is according to an embodiment of the present invention It is a flowchart showing the ultra-hardness TiAlSiN thin film deposition process using cathode arc deposition.

이를 참조하면, 본 발명의 일실시예에 따른 음극아크증착을 이용한 초고경도 TiAlSiN 박막 증착을 위한 음극아크 증착장치(2)는 Ti 타겟과, AlSi 타겟을 아크소스에 설치하여 질소 가스를 주입하면서 아크방전을 유기하여 플라즈마를 형성하여 피처리물의 표면에 TiAlSiN 코팅층을 형성하도록 함으로써 나노조직을 갖는 초고경도의 내마모성 절삭공구를 제조하는 방법이다.Referring to this, the cathode arc deposition apparatus 2 for depositing ultra-high hardness TiAlSiN thin film using cathode arc deposition according to an embodiment of the present invention is provided with a Ti target and an AlSi target in an arc source to inject nitrogen gas into the arc. It is a method for producing an ultra-hard wear-resistant cutting tool having a nanostructure by discharging the discharge to form a plasma to form a TiAlSiN coating layer on the surface of the workpiece.

보다 상세하게, 본 발명의 일실시예에 따른 음극아크증착을 이용한 초고경도 TiAlSiN 박막 증착을 위한 음극아크 증착장치(2)는 아크소스에 타겟을 부착하고 전압을 인가시켜 플라즈마를 발생시킴으로써 타겟에서 증발되는 물질이 플라즈마 내에서 이온화되어 피처리물에 증착되도록 하는 장치이다.More specifically, the cathode arc deposition apparatus 2 for ultra-hard TiAlSiN thin film deposition using cathode arc deposition according to an embodiment of the present invention attaches a target to an arc source and applies a voltage to evaporate from the target. The material to be ionized in the plasma to be deposited on the workpiece.

이러한 본 발명의 일실시예에 따른 음극아크증착을 이용한 초고경도 TiAlSiN 박막 증착을 위한 음극아크 증착장치(2)는 내부가 중공된 형태의 챔버(10)가 제공되며, 그 챔버(10)의 내벽면에는 아크 소스(12, 14)가 부착되어져 있으며, 그 아크소스(12, 14)에는 타겟 물질이 각각 결합되어져 있다The cathode arc deposition apparatus 2 for depositing ultra-high hardness TiAlSiN thin film using cathode arc deposition according to an embodiment of the present invention is provided with a chamber 10 having a hollow interior, and within the chamber 10. Arc sources 12 and 14 are attached to the wall, and target materials are respectively coupled to the arc sources 12 and 14, respectively.

제 1 아크소스(12)에는 Ti 타겟(11)이 결합되어져 있으며, 제 2 아크소스(14)에는 AlSi 타겟(13)이 결합되어져 있다. 제 1 아크소스(12)와 제 2 아크소스(14)에는 각각 아크전력 공급부(15, 16)가 전기적으로 접속되어져 그 아크소스(12, 14)로 전력을 공급하여 타겟(11, 13)으로부터 물질의 이온화가 이루어지도록 한다.The Ti target 11 is coupled to the first arc source 12, and the AlSi target 13 is coupled to the second arc source 14. The arc power supply units 15 and 16 are electrically connected to the first arc source 12 and the second arc source 14, respectively, to supply power to the arc sources 12 and 14, respectively, from the targets 11 and 13, respectively. Allow ionization of the material.

Ti 타겟(11)에 전력을 공급하는 아크전력 공급부(15)의 전위 및 전류는 14∼22V, 35∼55A 이며, AlSi 타겟(13)에 전력을 공급하는 아크전력 공급부(16)의 전위 및 전류는 15∼23V, 25∼55A 이며, 증착온도는 200∼450℃이다.The electric potential and current of the arc power supply unit 15 for supplying power to the Ti target 11 are 14 to 22 V and 35 to 55 A, and the electric potential and current of the arc power supply unit 16 for supplying power to the AlSi target 13. Is 15-23V, 25-55A, and vapor deposition temperature is 200-450 degreeC.

또한, 상기 챔버(10)의 다른 내벽면에는 피처리물 지지부(18)가 챔버(10)의 내벽면으로부터 연장되게 형성되어져 있으며, 그 피처리물 지지부(18)에는 그 피처리물의 오염물질을 제거하기 위해 에칭 전위를 제공하는 바이어스 전압/전력 공급부(24)와 전기적으로 접속되어져 있으며, 그 피처리물 지지부(18)에는 피처리물(17)이 결합되어져 있다. 상기 바이어스 전압/전력 공급부(24)에서의 바이어스 전압은 50∼400V이다.In addition, on the other inner wall surface of the chamber 10, the workpiece support portion 18 is formed to extend from the inner wall surface of the chamber 10, and the workpiece support portion 18 is provided with contaminants of the workpiece It is electrically connected to a bias voltage / power supply 24 that provides an etching potential for removal, and the workpiece 17 is coupled to the workpiece support 18. The bias voltage at the bias voltage / power supply unit 24 is 50 to 400V.

이때, 상기 피처리물(17)은 본 발명에서는 통상 SKD11 이라고 명명되어진 공구강 재질을 사용하였으나, 이에 한정되는 것은 아니고 초경합금이나 비철금속으로도 충분히 사용 가능하다.In this case, the workpiece 17 is generally used in the present invention, a tool steel material named SKD11, but is not limited thereto, and can be used as a cemented carbide or nonferrous metal.

또한, 상기 피처리물(17)에는 열전대(26)가 가까이 부착되어져 그 피처리물(17)의 온도를 실시간으로 검출하도록 되어 있으며, 그 열전대(26)는 온도조절기(25)로 해당 온도데이터를 인가시키도록 접속되어져 있어 설정온도로 조절하게 되어 있으며, 상기 바이어스 전압/전력 공급부(24)는 상기 피처리물(17)로 인가되는 전위를 조절하게 되어져 있다.In addition, a thermocouple 26 is closely attached to the workpiece 17 to detect the temperature of the workpiece 17 in real time, and the thermocouple 26 is a temperature controller 25 for the corresponding temperature data. The bias voltage / power supply unit 24 is adapted to adjust the potential applied to the object to be processed 17. The bias voltage / power supply unit 24 is connected to the set temperature.

따라서, 상기 Ti 타겟(11)과 AlSi 타겟(13)에 아크전력을 공급함으로써 이온화된 물질이 플라즈마를 형성하고, 그 플라즈마 상태의 물질이 상기 피처리물(17)에 음극 아크증착이 이루어지게 된다.Therefore, by supplying arc power to the Ti target 11 and the AlSi target 13, the ionized material forms a plasma, and the substance in the plasma state is subjected to cathode arc deposition on the workpiece 17. .

또한, 본 발명의 일실시예에 따른 음극아크증착을 이용한 초고경도 TiAlSiN 박막 증착을 위한 음극아크 증착장치(2)의 챔버(10)중 다른 내벽면에는 히터(19)가 구성되어져 있으며, 그 히터(19)는 전력공급부(21)가 각각 연결되어져 있으며, 공지의 배큐엠 게이지(20)는 함체에 연결되어 진공도를 측정하게 되어 있다.In addition, a heater 19 is configured on the other inner wall surface of the chamber 10 of the cathode arc deposition apparatus 2 for depositing ultra-hard TiAlSiN thin film using cathode arc deposition according to an embodiment of the present invention. 19, the power supply unit 21 is connected to each other, the known bacuem gauge 20 is connected to the enclosure to measure the degree of vacuum.

한편, 본 발명의 일실시예에 따른 음극아크증착을 이용한 초고경도 TiAlSiN 박막 증착을 위한 음극아크 증착장치(2)의 챔버(10)의 내벽 소정부에는 챔버(10) 내부의 오염공기를 배출시키기 위해 챔버(10) 내부의 공기를 제거하는 수단이 구비되는 바, 그 수단으로는 터보펌프(22)와 로타리펌프(23)가 함께 장착되어져 있고, 그 펌프들에 의해 챔버(10) 내부의 진공도가 10-5∼10-7 Torr로 낮춰지게 된다.On the other hand, to discharge the contaminated air inside the chamber 10 in the predetermined portion of the inner wall of the chamber 10 of the cathode arc deposition apparatus 2 for depositing ultra-high hardness TiAlSiN thin film using cathode arc deposition according to an embodiment of the present invention. In order to remove the air in the chamber 10, a means for removing the air is provided with a turbopump 22 and a rotary pump 23, and the pumps provide a vacuum inside the chamber 10. Is lowered to 10 -5 to 10 -7 Torr.

이하, 도 2를 참조하여, 본 발명의 일실시예에 따른 음극아크증착을 이용한 초고경도 TiAlSiN 박막 증착을 위한 음극아크 증착공정에 대해 설명한다.Hereinafter, a cathode arc deposition process for depositing ultra-high hardness TiAlSiN thin film using cathode arc deposition according to an embodiment of the present invention will be described with reference to FIG. 2.

음극아크증착을 이용한 초고경도 TiAlSiN 박막 증착을 위한 음극아크 증착공정은 크게 Ti타겟(11)과 AlSi 타겟(13) 혹은 TiAlSi 타겟(11,13)을 설치하는 타겟설치과정(제 1 단계: ST-1)과; 상기 타겟(11, 13) 및 피처리물(17)이 설치된 챔버(10) 내부의 진공도를 10-5∼10-7 Torr로 낮춰 상기 챔버(10) 내부의 공기를 제거하는 과정(제 2 단계: ST-2)과; 상기 챔버(10)로 불활성 가스를 주입하여 상기 챔버 내부의 진공도를 10-1∼10-3 Torr로 세팅하여 불활성 가스를 주입하는 과정(제 3 단계: ST-3)과; 질소(N)를 챔버(10)에 유입시킨 후 아크소스에 전류를 인가하여 플라즈마를 형성하고 바이어스 전압을 인가하여 TiAlSiN 층을 형성하는 과정(제 5 단계: ST-5)으로 이루어져 있다.Cathode arc deposition process for depositing ultra-hard TiAlSiN thin film using cathodic arc deposition is largely target installation process for installing Ti target 11 and AlSi target 13 or TiAlSi target 11,13 (Step 1: ST- 1) and; A process of removing air in the chamber 10 by lowering the vacuum degree in the chamber 10 in which the targets 11 and 13 and the workpiece 17 are installed to 10 -5 to 10 -7 Torr (second step) : ST-2); Injecting an inert gas into the chamber 10 to inject an inert gas by setting a vacuum degree within the chamber to 10 −1 to 10 −3 Torr (step 3: ST-3); After the nitrogen (N) is introduced into the chamber 10, a current is applied to the arc source to form a plasma, and a TiAlSiN layer is formed by applying a bias voltage (a fifth step: ST-5).

보다 상세하게, 상기 TiAlSiN 층을 형성하는 과정(제 5 단계: ST-5)에서 Ti 타겟(11)에 인가하는 전위는 18V∼22V 이고, 전류는 45∼65A이고, AlSi 타겟(13)에 인가하는 전위는 18V∼22V이고, 전류는 35A∼55A이며, TiAlSi 타겟에 인가하는 전위는 15∼25V이고 전류는 25∼45A이다.More specifically, in the process of forming the TiAlSiN layer (step 5: ST-5), the potential applied to the Ti target 11 is 18V to 22V, the current is 45 to 65A, and is applied to the AlSi target 13. The potential is 18V to 22V, the current is 35A to 55A, the potential to be applied to the TiAlSi target is 15 to 25V, and the current is 25 to 45A.

한편, 본 발명의 일실시예에 따른 음극아크증착을 이용한 초고경도 TiAlSiN 박막 증착을 위한 음극아크 증착공정에서는 상기 TiAlSiN 층을 형성하는 과정(제 5 단계: ST-5)의 전단계에서 피처리물(17)의 표면에 부착된 오염물질을 제거하기 위한 프리에칭 과정(제 4 단계: ST-4)이 더 포함될 수 있으며, 프리에칭 과정은 상기 피처리물(17)에만 에칭 전위 및 에칭 전류를 인가시킴으로써 챔버(10)내부의 진공도를 10-1∼10-2 Torr로 세팅되게 하고, 에칭전위는 310∼320V, 에칭전류는 0.6A가 되도록 하며, 프리에칭 과정은 약 10분간 프리에칭이 수행되도록 한다.On the other hand, in the cathode arc deposition process for depositing ultra-hard TiAlSiN thin film using the cathode arc deposition according to an embodiment of the present invention (5th step: ST-5) to be processed ( A pre-etching process (step 4: ST-4) may be further included to remove the contaminants attached to the surface of 17), and the pre-etching process applies an etching potential and an etching current only to the workpiece 17. By setting the vacuum degree in the chamber 10 to 10 -1 to 10 -2 Torr, the etching potential is 310 to 320V, the etching current is 0.6A, and the preetching process is performed for about 10 minutes. do.

상기한 과정을 통해 코팅된 상기 TiAlSiN 층은 나노 인덴터로 경도 측정을 행한 결과, 40∼50GPa의 경도를 얻을 수 있었으며, 밀착력은 스크래치 테스터로 측정한 결과 50N 이상의 임계하중을 얻었다.The TiAlSiN layer coated through the above process was measured with a nano indenter, and as a result, a hardness of 40-50 GPa was obtained, and the adhesion was measured with a scratch tester to obtain a critical load of 50 N or more.

도 3은 본 발명의 일실시예에 따른 음극아크증착을 이용한 초고경도 TiAlSiN 박막의 단면을 촬영한 전자현미경 사진이며, 도 4는 본 발명의 일실시예에 따른 음극아크증착을 이용한 초고경도 TiAlSiN 박막의 나노 경도를 측정한 도면이고, 도 5는 본 발명의 일실시예에 따른 음극아크증착을 이용한 초고경도 TiAlSiN 박막의 밀착력 시험결과를 나타내는 도면, 도 6은 본 발명의 일실시예에 따른 음극아크증착을 이용한 초고경도 TiAlSiN 박막의 전자현미경 표면 사진이다.3 is an electron micrograph showing a cross-section of the ultra-high hardness TiAlSiN thin film using a cathode arc deposition according to an embodiment of the present invention, Figure 4 is an ultra-hard TiAlSiN thin film using a cathode arc deposition according to an embodiment of the present invention 5 is a view measuring the nano hardness of, Figure 5 is a view showing the adhesion test results of the ultra-hardness TiAlSiN thin film using the negative electrode arc deposition according to an embodiment of the present invention, Figure 6 is a negative electrode arc according to an embodiment of the present invention Electron microscope surface photograph of ultra-hard TiAlSiN thin film using evaporation.

이를 참조하면, 본 발명의 일실시예에 따른 음극아크증착을 이용한 초고경도 TiAlSiN 박막은 도 2의 과정에 의해 코팅된 상기 TiAlSiN 층을 형성하게 되는 바, 본 실시예에서의 상기 Ti 타겟(11)에 인가되는 코팅전위는 18V이며, 코팅전류는 45A이고, AlSi 타겟(13)에 인가하는 코팅전위는 19V이고, 코팅전류는 35A를 적용하였다.Referring to this, the ultra-high hardness TiAlSiN thin film using the cathode arc deposition according to an embodiment of the present invention will form the TiAlSiN layer coated by the process of Figure 2, the Ti target 11 in the present embodiment The coating potential applied to was 18V, the coating current was 45A, the coating potential applied to the AlSi target 13 was 19V, and the coating current was 35A.

또한, 증착온도는 300℃, 바이어스 전압은 -150V를 사용하여 한시간 증착을 행하여 얻어진 TiAlSiN 박막의 파단면을 FE-SEM으로 촬영하여 도 3에 나타내었다. 도 3을 분석해보면 해당 TiAlSiN 박막의 파단면은 무정형으로 되어 있는 것을 알 수 있었다.In addition, the fracture surface of the TiAlSiN thin film obtained by carrying out deposition for one hour using 300 DEG C and a bias voltage of -150 V was photographed by FE-SEM and shown in FIG. 3, the fracture surface of the TiAlSiN thin film was found to be amorphous.

또한, TiAlSiN 박막의 Ti, Al, Si, N의 함량비는 Ti 50.03, Al 32.50, N 14.20, Si 3.03(wt.%) 정도 였으며, 불순물로서의 산소함량은 0.24% 정도였다.In addition, the Ti, Al, Si, N content ratio of the TiAlSiN thin film was about Ti 50.03, Al 32.50, N 14.20, Si 3.03 (wt.%), And the oxygen content as impurities was about 0.24%.

한편, TiAlSiN 박막의 경도는 나노인덴터로 측정한 결과를 도 4에 나타낸 바, 그 TiAlSiN 박막의 경도는 49GPa를 나타낼 정도로 초고경도화가 되었음을 알 수 있었다. 또한, 도 5에는 스크래치 테스터를 사용하여 상기 TiAlSiN 박막의 밀착력을 측정한 결과 52N의 임계하중을 얻었다. On the other hand, the hardness of the TiAlSiN thin film was measured with a nano indenter as shown in Figure 4, it was found that the hardness of the TiAlSiN thin film was extremely high enough to represent 49GPa. In addition, in FIG. 5, the adhesion force of the TiAlSiN thin film was measured using a scratch tester, thereby obtaining a critical load of 52N.

또, 도 6은 상기 TiAlSiN 박막을 전자현미경으로 촬상한 이미지인 바, 해당 이미지를 살펴보면 10nm의 나노 미세구조를 갖고 있음을 알 수 있었다.In addition, FIG. 6 shows an image obtained by capturing the TiAlSiN thin film under an electron microscope. As a result, the TiAlSiN thin film has a nanostructure of 10 nm.

또한, 본 발명의 실시예에 따른 음극아크증착을 이용한 초고경도 TiAlSiN 박막 증착방법은 TiAlSi 복합타겟을 아크소스에 설치하여 질소 가스를 주입하면서 아크방전을 유기하여 플라즈마를 형성하여 피처리물의 표면에 TiAlSiN 코팅층을 형성하도록 하는 경우에도 도 4, 5, 6에 도시된 결과치와 대동소이한 초고경도의 코팅박막을 얻을 수 있었으며, 본 발명의 실시예에 따른 음극아크증착을 이용한 초고경도 TiAlSiN 박막 증착방법은 바이어스 전압, 챔버 내부의 온도 등의 해당 설정범위에서 다소 허용 에러치를 감안하여 가변될 수도 있다.In addition, in the ultra-hardness TiAlSiN thin film deposition method using the cathode arc deposition according to an embodiment of the present invention, the TiAlSi composite target is installed in an arc source, injecting nitrogen gas to induce arc discharge to form a plasma to form TiAlSiN on the surface of the workpiece Even in the case of forming a coating layer, a coating film having an ultra-high hardness similar to the results shown in FIGS. 4, 5, and 6 was obtained, and the ultra-hardness TiAlSiN thin film deposition method using the cathode arc deposition according to the embodiment of the present invention It may be varied in consideration of an allowable error value in a corresponding setting range such as a bias voltage and a temperature inside the chamber.

한편, 본 발명의 실시예에 따른 음극아크증착을 이용한 초고경도 TiAlSiN 박막 증착방법은 단지 상기한 실시예에 한정되는 것이 아니라 그 기술적 요지를 이탈하지 않는 범위내에서 다양한 변경이 가능하다.On the other hand, the ultra-hardness TiAlSiN thin film deposition method using the cathode arc deposition according to an embodiment of the present invention is not limited to the above embodiments, but various modifications can be made within the scope without departing from the technical gist.

상기한 바와 같이, 본 발명에 따른 음극아크증착을 이용한 초고경도 TiAlSiN 박막 증착방법은 Ti 타겟에 인가되는 코팅전위는 18V이며, 코팅전류는 45A이고, AlSi 타겟에 인가하는 코팅전위는 19V이고, 코팅전류는 35A가 되도록 하여 음극 아크증착을 실시한 결과, 초고경도의 코팅박막을 얻게 되었다는 잇점이 있으며, 실제로 초경 엔드밀에 적용하여 절삭시험한 결과 TiAlN에 비해 5배의 경도를 얻게 된 장점이 있었다.As described above, in the ultra-hardness TiAlSiN thin film deposition method using the cathode arc deposition according to the present invention, the coating potential applied to the Ti target is 18V, the coating current is 45A, the coating potential applied to the AlSi target is 19V, and the coating As a result of conducting cathodic arc deposition with a current of 35 A, there was an advantage of obtaining an ultra-high hardness coating thin film. In fact, when applied to a carbide end mill, the cutting test resulted in a hardness of 5 times that of TiAlN.

도 1은 본 발명의 일실시예에 따른 음극아크증착을 이용한 초고경도 TiAlSiN 박막 증착을 행하기 위한 음극아크 증착장치의 구성을 개략적으로 도시한 모식도,1 is a schematic diagram schematically showing the configuration of a cathode arc deposition apparatus for performing ultra-hard TiAlSiN thin film deposition using a cathode arc deposition according to an embodiment of the present invention,

도 2는 본 발명의 일실시예에 따른 음극아크증착을 이용한 초고경도 TiAlSiN 박막 증착공정을 도시한 플로우챠트,2 is a flowchart illustrating a process of depositing an ultra-high hardness TiAlSiN thin film using cathode arc deposition according to an embodiment of the present invention;

도 3은 본 발명의 일실시예에 따른 음극아크증착을 이용한 초고경도 TiAlSiN 박막의 단면을 촬영한 전자현미경 사진,3 is an electron microscope photograph of a cross section of an ultra-hard TiAlSiN thin film using a cathode arc deposition according to an embodiment of the present invention,

도 4는 본 발명의 일실시예에 따른 음극아크증착을 이용한 초고경도 TiAlSiN 박막의 나노 경도를 측정한 도면,4 is a view measuring the nano-hardness of the ultra-high hardness TiAlSiN thin film using a cathode arc deposition according to an embodiment of the present invention,

도 5는 본 발명의 일실시예에 따른 음극아크증착을 이용한 초고경도 TiAlSiN 박막의 밀착력 시험결과를 나타내는 도면,5 is a view showing the adhesion test results of ultra-high hardness TiAlSiN thin film using the cathode arc deposition according to an embodiment of the present invention,

도 6은 본 발명의 일실시예에 따른 음극아크증착을 이용한 초고경도 TiAlSiN 박막의 전자현미경 표면 사진이다.6 is an electron microscope surface photograph of an ultra-high hardness TiAlSiN thin film using cathode arc deposition according to an embodiment of the present invention.

*도면의 주요부분에 대한 부호의 설명** Description of the symbols for the main parts of the drawings *

10:챔버, 11:Ti 타겟,10: chamber, 11: Ti target,

12,14:아크소스, 13:AlSi타겟,12, 14: Arcos, 13: AlSi target,

15,16:아크전력공급부, 17:피처리물,15, 16: arc power supply, 17: the workpiece,

18:피처리물지지대, 19:히터,18: workpiece support, 19: heater,

20:배큐엄게이지, 21:히터 전력공급부,20: back gauge, 21: heater power supply,

22:터보펌프, 23:로터리펌프,22: turbo pump, 23: rotary pump,

24:바이어스전압전력공급부, 25:온도조절기,24: bias voltage power supply, 25: temperature controller,

26:열전대.26: Thermocouple.

Claims (4)

음극아크증착을 이용한 초고경도 TiAlSiN 박막 증착을 위한 음극아크 증착공정은 크게 Ti타겟과 AlSi 타겟 혹은 TiAlSi 타겟을 설치하는 타겟설치과정과; Cathode arc deposition process for depositing ultra-hard TiAlSiN thin film using cathode arc deposition includes a target installation process for installing a Ti target and an AlSi target or a TiAlSi target; 상기 타겟들 및 피처리물이 설치된 챔버 내부의 진공도를 10-5∼10-7 Torr로 낮춰 상기 챔버 내부의 공기를 제거하는 과정과;Removing air in the chamber by lowering the degree of vacuum in the chamber in which the targets and the workpiece are installed to 10 −5 to 10 −7 Torr; 상기 챔버로 불활성 가스를 주입하여 상기 챔버 내부의 진공도를 10-1∼10-3 Torr로 세팅하여 피처리물 표면을 세정하는 플라즈마 클리닝 과정과;A plasma cleaning process of injecting an inert gas into the chamber to clean the surface of the workpiece by setting a vacuum degree within the chamber to 10 −1 to 10 −3 Torr; 질소를 챔버에 유입시킨 후 아크소스에 전류를 인가하여 플라즈마를 형성하고 바이어스 전압을 인가하여 TiAlSiN 층을 형성하는 과정으로 이루어진 것을 특징으로 하는 음극아크증착을 이용한 초고경도 TiAlSiN 박막 증착방법.A method of depositing ultra-hardness TiAlSiN thin film using cathode arc deposition, comprising: introducing nitrogen into a chamber, applying a current to an arc source to form a plasma, and applying a bias voltage to form a TiAlSiN layer. 제 1 항에 있어서, 상기 플라즈마 클리닝 과정은 에칭전위는 310∼320V, 에칭전류는 0.6A가 되도록 하며, 약 10분간 클리닝을 위한 에칭이 수행되도록 하는 것을 특징으로 하는 음극아크증착을 이용한 초고경도 TiAlSiN 박막 증착방법.The method of claim 1, wherein the plasma cleaning process has an etching potential of 310 to 320V, an etching current of 0.6A, and etching for cleaning for about 10 minutes is performed. Thin film deposition method. 제 1 항에 있어서, 상기 Ti 타겟에 공급되는 전위 및 전류는 14∼22V, 35∼55A 이며, AlSi 타겟에 공급되는 전위 및 전류는 15∼23V, 25∼55A 인 것을 특징으로 하는 음극아크증착을 이용한 초고경도 TiAlSiN 박막 증착방법.The cathode arc deposition according to claim 1, wherein the potential and current supplied to the Ti target are 14 to 22 V and 35 to 55 A, and the potential and current supplied to the AlSi target are 15 to 23 V and 25 to 55 A. Ultra-hardness TiAlSiN thin film deposition method using. 제 1 항에 있어서, 상기 Ti 타겟 및 AlSi 타겟의 피처리물에 대한 증착온도는 200∼450℃인 것을 특징으로 하는 음극아크증착을 이용한 초고경도 TiAlSiN 박막 증착방법.The method of claim 1, wherein the deposition target temperature of the Ti target and the AlSi target is about 200 ° C. to 450 ° C. The method of claim 1, wherein the Ti AlSiN thin film is deposited using cathode arc deposition.
KR1020050031701A 2005-04-16 2005-04-16 DEPOSITION OF SUPER HARD TiAlSiN THIN FILMS BY CATHODIC ARC PLASMA DEPOSITION KR100659743B1 (en)

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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR100758033B1 (en) * 2006-05-12 2007-09-11 울산대학교 산학협력단 Hard wear resistant thin films deposition device and method
KR100835387B1 (en) * 2006-09-19 2008-06-04 한국야금 주식회사 Cutting tool coated multi-element and multi-layer film with properties of high hardness and oxidation resistance at high temperature
CN109930106A (en) * 2019-05-08 2019-06-25 哈尔滨工业大学 A kind of preparation method of the TiAlSi/TiAlSiN multilayer alternate coatings with high wear resistance ability
CN113774347A (en) * 2021-09-14 2021-12-10 北京市辐射中心 Superhard and tough nano composite coating, preparation method and use equipment
WO2022225343A1 (en) * 2021-04-22 2022-10-27 스마트와이어 주식회사 Human soft tissue cutting wire, and method for manufacturing same

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR100758033B1 (en) * 2006-05-12 2007-09-11 울산대학교 산학협력단 Hard wear resistant thin films deposition device and method
KR100835387B1 (en) * 2006-09-19 2008-06-04 한국야금 주식회사 Cutting tool coated multi-element and multi-layer film with properties of high hardness and oxidation resistance at high temperature
CN109930106A (en) * 2019-05-08 2019-06-25 哈尔滨工业大学 A kind of preparation method of the TiAlSi/TiAlSiN multilayer alternate coatings with high wear resistance ability
WO2022225343A1 (en) * 2021-04-22 2022-10-27 스마트와이어 주식회사 Human soft tissue cutting wire, and method for manufacturing same
CN113774347A (en) * 2021-09-14 2021-12-10 北京市辐射中心 Superhard and tough nano composite coating, preparation method and use equipment

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