WO2020230994A1 - Film de revêtement nanométrique dur multicouche pour outil de formation en forme de dent - Google Patents

Film de revêtement nanométrique dur multicouche pour outil de formation en forme de dent Download PDF

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Publication number
WO2020230994A1
WO2020230994A1 PCT/KR2020/003738 KR2020003738W WO2020230994A1 WO 2020230994 A1 WO2020230994 A1 WO 2020230994A1 KR 2020003738 W KR2020003738 W KR 2020003738W WO 2020230994 A1 WO2020230994 A1 WO 2020230994A1
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layer
coating film
hard coating
multilayer nano
tool
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PCT/KR2020/003738
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English (en)
Korean (ko)
Inventor
이병열
서형권
김용희
이미경
윤수경
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주식회사 다올플라즈마
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Publication of WO2020230994A1 publication Critical patent/WO2020230994A1/fr

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    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
    • C23C14/0641—Nitrides
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
    • C23C14/24—Vacuum evaporation
    • C23C14/32—Vacuum evaporation by explosion; by evaporation and subsequent ionisation of the vapours, e.g. ion-plating
    • C23C14/325—Electric arc evaporation
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C28/00—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D
    • C23C28/04—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D only coatings of inorganic non-metallic material
    • C23C28/044—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D only coatings of inorganic non-metallic material coatings specially adapted for cutting tools or wear applications
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C28/00—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D
    • C23C28/40—Coatings including alternating layers following a pattern, a periodic or defined repetition
    • C23C28/44—Coatings including alternating layers following a pattern, a periodic or defined repetition characterized by a measurable physical property of the alternating layer or system, e.g. thickness, density, hardness

Definitions

  • the present invention relates to a multi-layer nano hard coating film for a forming tooth tool, and more particularly, to a multi-layer nano hard coating film for forming tooth tool having a composite multi-layer structure on nano-ized coating particles to improve the abrasion resistance and life characteristics of the forming tooth tool.
  • a multi-layer nano hard coating film for a forming tooth tool and more particularly, to a multi-layer nano hard coating film for forming tooth tool having a composite multi-layer structure on nano-ized coating particles to improve the abrasion resistance and life characteristics of the forming tooth tool.
  • the tool In order to improve the performance of the tool, it is mainly made of high-quality materials such as fine powder alloy carbide, cermet, or powdered high-speed steel, and is designed in an optimal shape and surface coating is applied to improve life.
  • high-quality materials such as fine powder alloy carbide, cermet, or powdered high-speed steel
  • PVD physical vapor deposition
  • CVD chemical vapor deposition
  • TiAlN coating by physical vapor deposition is widely used as a method for wear prevention application.
  • European Patent No. 1173528 discloses a technique for a coating film consisting of a plurality of individual layers for a tool.
  • the first layer of the technology is made of nitride, carbide, carbonitride, boride, oxide, etc. of the elements Ti, Al and or Cr
  • the second layer includes at least one Si and periodic table IVa, Va and VIa groups It is made of elemental nitride, carbide, carbonitride, boride, oxide, etc., and such a coating film is advantageous in that abrasion resistance and oxidation resistance are significantly improved by Si in the upper layer.
  • a cover layer based on Cr-Si is It is characterized by improved longevity.
  • a TiAlN-layer, a CrAlN-layer, and a TiN-layer are selected as lower layers.
  • European Patent No. 1422311 Hard film and hard film coated tool
  • a hard material layer based on Al-Cr-(Si)-O
  • the material layer is nitride, carbide, oxide, It can be configured as boride or the like.
  • This technique applies to all layers that a small amount of oxygen content (1 to 25 atomic%) is contained in the layer, and an additional hard material layer can be applied to the coating film, in particular Ti-Si-N, Ti -BN, Cr-Si-N, etc. are presented.
  • an advantage of this technique mention is made, in particular, of oxygen or a small amount of acceptance of silicon and oxygen, since this leads to a higher hardness as well as improved abrasion resistance and high temperature oxidation resistance.
  • European Patent No. 1219723 Hard film for cutting tools
  • a coating film based on Ti-Al-Cr-X-N where X may represent Si, B and/or C.
  • wear resistance is improved compared to a conventional coating film, and it is described that it should be made of at least Ti, Al, and Cr.
  • a hard material coating film based on Ti-Al-N or Al-Cr-N has a short lasting life.
  • the coating film according to the prior art in the case of the Al-Cr-N coating layer, has a disadvantage that the decomposition of the coating film is already started at about 900° C. under an inert gas atmosphere (eg, argon atmosphere) at a high temperature.
  • an inert gas atmosphere eg, argon atmosphere
  • the decomposition step moves to a higher temperature range, especially when considering a continuous step in the chipping process, locally exceeds 1000°C at the contact surface between the tool surface and the product. Very high temperatures occur. Therefore, if the contact surface is large enough so that oxygen cannot act stably at all/almost on the surface of the coating film, the Cubic CrN is decayed into hexagonal Cr2N and in a subsequent step at a higher temperature, such a coating film The decomposition process leads to premature wear of the coating film.
  • the present invention was conceived to solve the above problems, and an object of the present invention is a multi-layer for forming tooth tool deposited to have a composite multi-layer structure on nano-coated particles in order to improve the tool life of the forming tooth tool It is to provide a nano hard coating film.
  • another object of the present invention is to provide a multilayer nano hard coating film for a forming tooth tool having a special multilayer structure in order to prevent rapid decomposition (wear) of the coating film in the use of the tool.
  • the present invention provides a multilayer nano hard coating film for a forming tooth tool in order to achieve the above object, comprising: a first layer having a composition of the following formula (1) formed on a metal substrate layer which is a forming tooth tool; A second layer formed on an upper surface of the first layer and having a mixed composition of the following formula 1 and the following formula 2; And a third layer having a composition of the following formula (2) formed on the upper surface of the second layer; it is possible to provide a multilayer nano hard coating film, characterized in that it is continuously repeatedly formed.
  • X represents one of the group consisting of N, CN, BN, NO, CNO, CBN, BNO and CNBO
  • Me is V, Nd, Sm, Eu, Hf, In, Sn, Zr, Ta, W, Nb It represents one of the crowds consisting of, and a, b, u, v, and w represent the stoichiometric composition of the target part.
  • a thickness ratio of the second layer or the third layer to the first layer is greater than 0.5.
  • the first layer, the second layer, or the third layer may be deposited by performing any one of an ion gun etching process, a halo cathode etching process, and a metal ion etching process.
  • the first layer, the second layer, or the third layer is deposited by applying a negative bias voltage of 35 to 300V, but is deposited by applying the negative bias voltage in a stepwise manner over time. To do.
  • the present invention has the advantage of improving the tool life of products such as tooth pin manufacturing tools, cutting and forming tools, or machining devices and parts.
  • the present invention has the advantage that the hard coating film has a special multilayer structure, so that rapid decomposition (wear) of the coating film can be prevented in the use of a tool, and the wear resistance life of the coating film can be increased by imparting lubricating properties. have.
  • FIG. 1 is a view showing the structure of a multilayer nano hard coating film for a forming tooth tool according to the present invention.
  • Figure 2 is a photograph showing the structure of the multilayer nano-hard coating film for a forming tooth tool according to the present invention.
  • FIG 3 is a plan view schematically illustrating a vacuum deposition chamber shown as an exemplary embodiment of the present invention.
  • Multilayer nano hard coating film according to the present invention is a tool, a machining tool, a forming and chippin processing tool, a milling tool, a cutting tool, a turning tool, a tapping tool, and a reamer. It can be applied to improve wear resistance and life characteristics of (Reamer), Endmill, Drill, Cutting Insert, Gear Cutting Tool, Insert, Hob, Cutter, etc. ,
  • a forming tooth tool the following describes a multilayer nano-hard coating film for a forming tooth tool according to the present invention, but this is only an example to aid understanding of the present invention, and the scope of the present invention is limited thereto It does not become.
  • FIG. 1 is a view showing the structure of a multi-layer nano hard coating film for a forming tooth tool according to the present invention
  • Figure 2 is a photograph showing the structure of the multi-layer nano hard coating film for a forming tooth tool according to the present invention.
  • the first layer formed on the metal substrate layer, which is a forming tooth tool, the second layer formed on the upper surface of the first layer, and the third layer formed on the upper surface of the second layer are continuously repeated. Is formed.
  • the first layer It has a composition of
  • the third layer is And the second layer for improved adhesion between the first layer and the third layer and It has a mixed composition of, and the first to third layers are sequentially stacked and formed, and it is preferable that the hard coating layer is repeatedly formed 8 or more times to improve the performance.
  • X represents one of the group consisting of N, CN, BN, NO, CNO, CBN, BNO and CNBO, preferably N or CN, and more preferably N.
  • Me represents one or a mixture of two or more of the group consisting of V, Nd, Sm, Eu, Hf, In, Sn, Zr, Ta, W, and Nb, and a, b, u, v, w are the target portion. Represent stoichiometric composition.
  • a is 0.5 ⁇ a ⁇ 0.7
  • b is 0.05 ⁇ b ⁇ 0.1
  • u is 0.5 ⁇ u ⁇ 0.7
  • v is 0.02 ⁇ v ⁇ 0.08, and w is 0.01 ⁇ w ⁇ 0.08.
  • the first layer, the second layer, or the third layer may be deposited by performing at least one selected from an ion gun etching process, a halo cathode etching process, and a metal ion etching process, and the first layer or The third layer has a microcrystalline form having an average particle size of about 5 to 150 nm, preferably 10 to 120 nm.
  • the thickness ratio of the second layer or the third layer to the first layer is set to exceed 0.5.
  • the second layer or the third layer includes two or more crystalline phases, and preferably, an equiaxed crystal system and a hexagonal crystal system).
  • the hard coating film is a cube And the first layer of, and Of the second layer of the mixed composition of and the cube
  • the third layer of is alternately deposited to have a multi-layered structure, as shown in FIG. 2, the thickness is uniform and the possibility of occurrence of defects such as cracks is significantly reduced to have a dense structure. Can improve.
  • the hard coating film is applied with a negative bias voltage of 35 to 300V in order to further improve the wear resistance and life characteristics of the forming tooth tool, but the bias voltage is increased stepwise with time, and applied for each step section. It is formed by evaporation, and a detailed description thereof will be described later.
  • FIG 3 is a plan view schematically illustrating a vacuum deposition chamber according to an exemplary embodiment of the present invention.
  • the hard coating film that is, the Al-Cr-SiN/AlTiMoMeN hard layers
  • an AIP type industrial coating facility of ISYS is used.
  • the refined forming tooth tool is fixed on a double rotary substrate carrier according to the diameter, or on a triple rotary substrate carrier for a diameter of less than 50 mm, and a target made of an Al-Cr-Si alloy manufactured by powder metal metallurgy. And a target made of an Al-Ti-Mo-Me alloy is placed in twelve cathode arc power sources provided on the walls of the coating installation as shown in FIG. 3.
  • the targets disposed in the first to third negative arc power sources (1, 2, 3) and the seventh to ninth negative arc power sources (7, 8, 9) are targets made of Al-Cr-Si alloy, and 4
  • the targets disposed in the sixth to sixth negative arc power supply (4, 5, 6) and the seventh to ninth negative arc power supply (10, 11, 12) is preferably a target made of an Al-Ti-Mo-Me alloy, It is not limited to this.
  • the geometry of the target arrangement is substantially determined by the octagonal plan view of the AIP type industrial coating facility, and is disposed within the intermediate element of each ternary group, but is not limited thereto, and the first to third layers are manufactured. Other target placements are also possible.
  • the second layer is additionally deposited with a multi-layered structure having a very delicate layer due to the rotation of the product during deposition due to the geometric target arrangement of the coating facility.
  • Al-Cr-Si and Al-Ti-Mo-Me Since individual targets based are used to form the coating film, the width of the second layer is changed in the range of several nanometers.
  • first to third layers may be deposited at the same coating layer height of a single rotational or multiple rotational substrate fixing device, and preferably in all installations including at least three arc cathodes at geometrically equivalent positions. Can be deposited.
  • the operator can influence the layer thickness or position of each layer by the placement of the target according to each type of equipment, and also, the control of the movement or rotation of each substrate, or the angular velocity of product rotation. By affecting the layer thickness or location of individual layers.
  • the foaming tooth tool which is a product to be coated, is provided at a temperature of about 500°C in a radiant heating device provided in the facility, and the surface is then subjected to a pressure of 0.2Pa by application of a DC-bias voltage of -300 to -600V under Ar atmosphere. It is provided through an etching purification process by Ar ions and a hollow cathode ion cleaning process.
  • Al-Cr-Si-N hard layer of about 0.2 mu m thickness was deposited by operation of six Al-Cr-Si power supplies using 80A output and application of a voltage of -35V substrate bias for about 5 minutes.
  • a multilayer is intentionally formed.
  • an additional six Al-Ti-Mo-Me power supplies are similarly switched on to 150A each, and a substrate bias of -150V for about 3 minutes. It is operated jointly by applying voltage.
  • six Al-Cr-Si power supplies are switched off and only an Al-Ti-Mo-Me-N coating layer is deposited by applying a substrate bias voltage of -300V for about 3 minutes.
  • This stepwise voltage application process is repeatedly performed eight times during the deposition process within the scope of the present invention, and all layers are deposited at a pressure of about 40 mtorr and a negative substrate bias voltage of about 35V to 300V in a pure nitrogen (N) atmosphere.
  • Comparative Example 1 is a target made of an Al-Cr alloy having a composition of 60 atomic% Al and 40 atomic% Cr, as shown in Table 1, and an Al-Ti- having a composition of 67 atomic% Al, 31 atomic% Ti and 2 atomic% Mo. It is a coating film deposited with a target made of Mo alloy.
  • Comparative Example 1 was a ⁇ 127mm, a 15T disk type (disc type) target was used.
  • Example 1 the target composition of the layer forming the coating film was different, and the coating film was formed according to the target performance of Table 2, the process parameters such as the minor substrate bias voltage, the process pressure and temperature. .
  • the target used in Examples 1 to 9 is a ⁇ 127mm, 15T disk type target, as shown in FIG. 3, the first to third negative arc power sources (1, 2, 3) And the 7th to ninth negative arc power source (7, 8, 9) was arranged to insert a target made of an Al-Cr-Si alloy, the fourth to sixth negative arc power source (4, 5, 6) and the 7th to Targets made of an Al-Ti-Mo-Me alloy were inserted into the ninth cathode arc power sources 10, 11, and 12.
  • the thickness, hardness, adhesion and roughness of each of the hard coating films of Examples 1 to 9 were measured and shown in Table 3.
  • the thickness of the hard coating film was measured by a Calotest, and the hardness was measured by a Vickers hardness tester. Tester).
  • the adhesion of the hard coating film was measured by a scratch test, and the measured roughness is an arithmetic average roughness (Ra), and the unit is micrometer ( ⁇ m).
  • Example 1 Number of times result thickness Hardness (Hv) Adhesion (N) Illuminance (Ra( ⁇ m)) Comparative Example 1 4.5 3,241.4 78.1 0.11
  • Example 1 5.2 3,369.2 80 0.09
  • Example 2 5.4 3,312.7 80 0.10
  • Example 3 4.7 3,431.8 80 0.18
  • Example 4 5.6 3,285.6 80 0.12
  • Example 5 5.0 3,342.7 80 0.10
  • Example 6 5.3 3,542.3 80 0.11
  • Example 7 6.2 3,489.6 80 0.11
  • Examples 1 to 7 which are coating films deposited with a target made of an Al-Cr-Si alloy and a target made of an Al-Ti-Mo-Me alloy, are a target made of an Al-Cr alloy and an Al-Ti It was confirmed that the thickness of the coating film was increased compared to Comparative Example 1, which is a coating film deposited with a target made of -Mo alloy, and adhesion and hardness were also improved.

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Physical Vapour Deposition (AREA)
  • Cutting Tools, Boring Holders, And Turrets (AREA)

Abstract

La présente invention concerne un film de revêtement nanométrique dur multicouche pour un outil de formation en forme de dent, et plus spécifiquement, un film de revêtement nanométrique multicouche pour un outil de formation en forme de dent, des particules de revêtement de taille nanométrique étant disposées dans une structure multicouche composite afin d'améliorer les caractéristiques de résistance à l'usure et de durée de vie de l'outil de formation en forme de dent.
PCT/KR2020/003738 2019-05-13 2020-03-19 Film de revêtement nanométrique dur multicouche pour outil de formation en forme de dent WO2020230994A1 (fr)

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KR1020190055948A KR102074469B1 (ko) 2019-05-13 2019-05-13 포밍 치형공구용 다층나노 경질 코팅막
KR10-2019-0055948 2019-05-13

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CN115216726A (zh) * 2022-08-24 2022-10-21 烟台佳隆纳米产业有限公司 高性能薄膜材料及其制备方法

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KR102074469B1 (ko) * 2019-05-13 2020-02-07 주식회사 다올플라즈마 포밍 치형공구용 다층나노 경질 코팅막
KR102577510B1 (ko) * 2021-05-25 2023-09-12 주식회사 다올플라즈마 수명이 향상된 키홈 제작 공구

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JP2006082209A (ja) * 2004-09-17 2006-03-30 Sumitomo Electric Hardmetal Corp 表面被覆切削工具
JP2007191765A (ja) * 2006-01-20 2007-08-02 Kobe Steel Ltd 硬質皮膜
KR20080061323A (ko) * 2006-12-27 2008-07-02 산드빅 인터렉츄얼 프로퍼티 에이비 다층 피복 절삭 공구
KR101616600B1 (ko) * 2009-11-12 2016-04-28 오에스지 가부시키가이샤 경질 피막 피복 공구
US20160194748A1 (en) * 2012-09-04 2016-07-07 FoxyLED GmbH Coated cutting tool and a method for coating the cutting tool
KR102074469B1 (ko) * 2019-05-13 2020-02-07 주식회사 다올플라즈마 포밍 치형공구용 다층나노 경질 코팅막

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN115216726A (zh) * 2022-08-24 2022-10-21 烟台佳隆纳米产业有限公司 高性能薄膜材料及其制备方法
CN115216726B (zh) * 2022-08-24 2023-11-14 烟台佳隆纳米产业有限公司 高性能薄膜材料及其制备方法

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