KR20010027790A - Multilayer ion-coating method being fluorine compound on metal surface - Google Patents

Multilayer ion-coating method being fluorine compound on metal surface Download PDF

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KR20010027790A
KR20010027790A KR1019990039700A KR19990039700A KR20010027790A KR 20010027790 A KR20010027790 A KR 20010027790A KR 1019990039700 A KR1019990039700 A KR 1019990039700A KR 19990039700 A KR19990039700 A KR 19990039700A KR 20010027790 A KR20010027790 A KR 20010027790A
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layer
tialn
ion plating
plated layer
gas
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KR100321613B1 (en
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박종천
최인식
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권문구
엘지전선 주식회사
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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
    • 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
    • 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
    • C23C8/00—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
    • C23C8/06—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using gases
    • C23C8/08—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using gases only one element being applied
    • 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
    • C23C8/00—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
    • C23C8/06—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using gases
    • C23C8/08—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using gases only one element being applied
    • C23C8/10—Oxidising
    • C23C8/12—Oxidising using elemental oxygen or ozone
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
    • B23B—TURNING; BORING
    • B23B2228/00—Properties of materials of tools or workpieces, materials of tools or workpieces applied in a specific manner
    • B23B2228/10—Coatings

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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)
  • Chemical Vapour Deposition (AREA)

Abstract

PURPOSE: A method for plating multi-layered ion comprising fluoride on surface of a metal is provided to improve and increase hardness, abrasion resistance and life cycle of a high speed cutting tool by treating a multi-layered ion plating comprising fluorides such as AlF3, Al(FxOy)n, etc. on surface of the metal so that oxidation of a cutting tool or a metal component is prevented under the fluorine gas environment. CONSTITUTION: The multi-layered ion plating method comprises the processes of ion plating TiAlN on a cutting tool or surface of a metal exposed to HF gas in PEPVD (Plasma Enhanced Physical Vapor Deposition) method or PECVD (Plasma Enhanced Chemical Vapor Deposition) method, forming an Al2O3 layer on surface of the plated layer by exposing the plated layer to air of 200 to 400 deg.C for 1 to 3 hours, and forming an Al2F3 layer or an Al(FxOy)n layer on surface of the plated layer by exposing the plated layer under the HF gas environment of 350 to 400 deg.C for 1 to 6 hours. The multi-layered ion plating method comprises the process of forming an Al2F3 layer or an Al(FxOy)n layer on surface of the TiAlN plated layer by exposing the TiAlN plated layer to the mixture of air having a temperature of 350 to 400 deg.C and HF gas for 1 to 6 hours after the TiAlN ion plating.

Description

금속표면에 불소화합물을 포함하는 다층 이온도금 방법{MULTILAYER ION-COATING METHOD BEING FLUORINE COMPOUND ON METAL SURFACE}Multi-layer ion plating method containing fluorine compound on metal surface {MULTILAYER ION-COATING METHOD BEING FLUORINE COMPOUND ON METAL SURFACE}

본 발명은 금속표면에 다층 이온도금하는 방법에 관한 것으로, 특히 금속 표면에 ΑlＦ3, Al(ＦχＯy)n등의 불소화합물을 포함하는 다층 이온도금 처리하여 불소가스 분위기 하에서의 절삭공구나 금속 부품의 산화방지를 가능하게 한 금속표면에 불소화합물을 포함하는 다층 이온도금 방법에 관한 것이다.BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a method of multi-layer ion plating on a metal surface, and more particularly, to cutting metals or metals in a fluorine gas atmosphere by applying a multi-layer ion plating process containing fluorine compounds such as AlF 3 and Al (F x O y ) n on the metal surface. The present invention relates to a multi-layer ion plating method comprising a fluorine compound on a metal surface that enables oxidation prevention of a part.

일반적으로 건식도금에 사용되는 기술에는 PVD(Physical Vapor Deposition)법과 CVD(Chemical Vapor Deposition)법이 있고, 여기에 플라즈마를 첨가시킨 이온도금 방법으로 PEPVD(Plasma Enhenced PVD)법과 PECVD(Plasma Enhenced CVD)법이 알려져 있다.In general, the techniques used for dry plating include PVD (Physical Vapor Deposition) and CVD (Chemical Vapor Deposition). Plasma-added ion plating methods are PEPVD (Plasma Enhenced PVD) and PECVD (Plasma Enhenced CVD) methods. This is known.

이와 같은 방법들을 활용하면 합금강 표면에 내마모성을 증가시키기 위해 질화티탄(TiN) 등을 도금하며, 이중 고온·고속 절삭공구의 수명을 높이기 위한 대표적인 이온도금 방법은 질화알루미늄티탄(TiAlN) 도금이다.By utilizing these methods, titanium nitride (TiN) is plated on the surface of the alloy steel to increase wear resistance, and a typical ion plating method for increasing the life of high temperature and high speed cutting tools is aluminum titanium nitride (TiAlN) plating.

TiAlN 도금층은 내마모성이 우수하고 경도가 매우 높으며 200∼400℃에서도 TiAlN중의 Al원소가 공기중의 산소와 반응하여 표면에 치밀한 산화알루미늄(Al2O3) 형성으로 내식성을 갖는다. 또한 치밀하게 형성된 Al2O2층의 보호로 TiAlN 도금층은 온도가 800℃까지 국부적으로 올라가도 수분정도의 시간은 견디므로 절삭공구에 TiAlN을 도금하면 경도가 높고 열처리된 강도 고속절삭 가공이 가능하다.The TiAlN plating layer has excellent abrasion resistance and very high hardness, and even at 200 to 400 ° C., the Al element in TiAlN reacts with oxygen in the air to form a dense aluminum oxide (Al 2 O 3 ) on the surface to provide corrosion resistance. In addition, the TiAlN plated layer withstands the moisture level even when the temperature is locally raised to 800 ℃ due to the protection of the densely formed Al 2 O 2 layer. Therefore, if TiAlN is plated on the cutting tool, the hardness is high and the heat treatment strength is possible.

그런데 금속소재 표면에 TiAlN만 도금된 상태에서는 도금층의 접촉 온도가 800℃ 이상이 되면 다층 도금층이 분해되고, 경도가 떨어지며 내마모성이 취약해지므로 고속 절삭공구의 수명이 단축된다.However, in the state where only TiAlN is plated on the surface of the metal material, when the contact temperature of the plated layer is 800 ° C. or more, the multilayer plated layer is decomposed, the hardness decreases, and the wear resistance becomes weak, thereby shortening the life of the high speed cutting tool.

더욱이 이렇게 되면, 테프론(Teflon)피복전선을 압출하는데 사용하는 압출기의 주요 부품 예컨데, 스크류, 다이 및 니플에 TiAlN만 도금된 상태에서는 도금에 악영향을 주어 피복전선의 표면이 매끄럽지 못한 불량을 유발하는 원인이 되기도 한다.Furthermore, this causes major parts of the extruder used to extrude Teflon-coated wires, for example, when TiAlN is plated only on screws, dies and nipples, which adversely affects the plating and causes the surface of the coated wires to be unsmooth. It can also be.

따라서 본 발명은 800℃ 이상의 대기중 온도에서 TiTlN 도금층이 수분 보다 더욱 긴 시간동안 견딜 수 있게 하여 절삭공구나 금속부품의 수명을 종래보다 더욱 증가시키기 위한 금속표면에 불소화합물을 포함하는 다층 이온도금 방법을 제공함에 그 목적이 있다.Therefore, the present invention is a multi-layer ion plating method comprising a fluorine compound on the metal surface to allow the TiTlN plated layer to withstand a longer time than the moisture at 800 ℃ or more in the air to further increase the life of cutting tools or metal parts than conventional The purpose is to provide.

상기의 목적을 달성하기 위한 본 발명의 구체적인 수단은,Specific means of the present invention for achieving the above object,

절삭공구 또는 HF 가스에 노출되는 금속표면에 PEPVD 혹은 PECVD 방법으로 TiTlN을 이온 도금한 후 200∼400℃의 대기중에 1∼3시간 동안 노출시켜 도금층 표면에 Al2O3층을 형성시킨 후 350∼400℃의 HF 가스 분위기 하에 1∼6시간 동안 노출시켜 도금층 표면에 AlF3나 Al(FXOY)N층을 형성시키는 것을 특징으로 한다.TiTlN was ion-plated on the metal surface exposed to the cutting tool or HF gas by PEPVD or PECVD, and then exposed for 1 to 3 hours in the atmosphere at 200 to 400 ° C to form an Al 2 O 3 layer on the surface of the plating layer. It is characterized by forming an AlF 3 or Al (F X O Y ) N layer on the surface of the plating layer by exposing for 1 to 6 hours in an HF gas atmosphere of 400 ℃.

이하, 본 발명의 실시예를 상세히 설명한다.Hereinafter, embodiments of the present invention will be described in detail.

본 발명은 절삭공구 또는 주요 금속부품에 PEPVD 혹은 PECVD 방법으로 TiAlN을 이온 도금한 후 200∼400℃의 대기중에 1∼3시간 동안 인위적으로 노출시키면 TiAlN 이온도금층이 산화되어 도금층 표면에 1차적으로 Al2O3가 형성된다. 즉, 산화전처리(Pre-oxidation) 과정을 밟는다.According to the present invention, when TiAlN is ion plated to a cutting tool or a main metal part by PEPVD or PECVD, and artificially exposed to air at 200 to 400 ° C. for 1 to 3 hours, the TiAlN ion plating layer is oxidized and Al is primarily on the surface of the plating layer. 2 O 3 is formed. That is, the pre-oxidation process is performed.

산화전처리의 층을 형성시킨 후 350∼400℃의 HF(플루오르화수소산) 가스 분위기 하에 1∼6시간 동안 노출시키면, Al2O3의 산소가 HF 가스중의 불소와 치환되어 역시 치밀한 AlF3가 형성된다.After forming the pre-oxidation layer and exposing for 1 to 6 hours in an HF (hydrofluoric acid) gas atmosphere at 350 to 400 ° C., oxygen of Al 2 O 3 is substituted with fluorine in HF gas to further form dense AlF 3 . Is formed.

또한 TiAlN 층의 Al과 HF 가스중의 불소가 반응하여 역시 AlF3가 생성되며, 대기중이므로 Al(FXOY)가 생성되기도 한다.In addition, AlF 3 is generated by reacting Al in the TiAlN layer with fluorine in HF gas, and Al (F X O Y ) is also generated because it is in the atmosphere.

이때 Al(FXOY)N에서 x + y = 1이며, n은 2.3∼3의 숫자를 갖는다.At this time, x + y = 1 in Al (F X O Y ) N , n has a number of 2.3 to 3.

이렇게 하여 금속 표면에 치밀하게 생성된 AlF3혹은 Al(FXOY)N은 1200℃까지도 대기중에서도 분해되지 않고 안정하며, 경도가 높고 산이나 알카리에도 침식되지 않으며, 특히 불산(Hydrofluoric acid)에도 침식되지 않는다.In this way, AlF 3 or Al (F X O Y ) N which is formed on the metal surface is not decomposed and stable even in the atmosphere up to 1200 ° C, and its hardness is high, and it does not corrode in acid or alkali, especially in hydrofluoric acid. Does not erode

따라서 위에서 기술한 방법으로 TiAlN 도금층 위에 AlF3나 Al(FXOY)N층을 생성시켜 다층 도금층(Multilayer)을 형성시키면 종래 방법에 의한 것이 최대 사용온도가 800℃인데 비하여 본 발명이 방법에 의해 표면처리된 것은 800℃ 보다 높은 900℃에서도 다층 도금층이 분해되지 않고 견디고, 높은 경도가 유지되어 내마모성이 우수하므로 고속 절삭공구 등 공구의 수명을 10배 이상 연장할 수 있다.Therefore, by forming the AlF 3 or Al (F X O Y ) N layer on the TiAlN plated layer by the above-described method to form a multi-layer plated layer (Multilayer), the present invention has a maximum operating temperature of 800 ℃ The surface-treated by the multilayered coating layer is resistant to decomposition even at 900 ℃ higher than 800 ℃, high hardness is maintained and wear resistance is excellent, it is possible to extend the life of tools such as high-speed cutting tools more than 10 times.

또한 AlF3나 Al(FXOY)N은 플루오르화수소산 가스(HF gas) 분위기에서도 400℃까지 분해되지 않고 견딘다.In addition, AlF 3 or Al (F X O Y ) N withstands up to 400 ℃ even in the hydrofluoric acid gas (HF gas) atmosphere.

한편, 테프론(Teflon) 피복전선을 압출제조 할 경우에는 전술한 바와 같이 압출온도가 300∼400℃로 높으며 이때, 테프론 수지로부터 분해된 HF 가스가 발생하여 압출기 주요 부품인 스크류(screw), 다이(die) 및 니플(nipple)이 일반 합금강이면 이들을 심하게 부식시키므로 테프론 피복전선용 압출기의 스크류, 다이 및 니플은 HF가스에 부식이 잘 안되는 하스텔로이(Hastelloy) 등을 종래에는 사용하고 있다.On the other hand, when extruded Teflon-coated wire as described above, the extrusion temperature is as high as 300 ~ 400 ℃, at this time, HF gas decomposed from the Teflon resin is generated, screw, die ( If the die and the nipple are ordinary alloy steels, they are severely corroded. Thus, the screws, dies, and nipples of the extruder for Teflon-coated wires have conventionally used Hastelloy, etc., which are hardly corroded to HF gas.

그러나 하스텔로이는 가격이 고가일뿐더러 경도가 낮아 마모가 잘되어 수명이 짧은 단점을 가지고 있다.However, Hastelloy has the disadvantage that the price is high and the hardness is low, so wear is good and the life is short.

따라서 테프론 피복전선용 압출기의 스크류, 다이 및 니플 등 주요 부품을 본 발명의 방법으로 표면처리하면, 주요 부품의 수명을 10배 이상 연장할 수 있는 것으로 나타났다.Therefore, surface treatment of the main parts such as screw, die and nipple of the extruder for Teflon coated wire by the method of the present invention, it was found that the life of the main parts can be extended by more than 10 times.

또한 AlF3나 Al(FXOY)N도금층과 용융된 테프론 레진과의 접착력이 하스텔로이와 용융된 테프론 레진과의 접착력보다 작으므로 본 발명 방법에 의해 주요 부품을 처리하여 테프론 피복 전선을 압출하면 윤활성이 좋아 압출된 피복전선은 표면이 매끄러운 장점을 갖는다.In addition, since the adhesion between the AlF 3 or Al (F X O Y ) N plated layer and the molten Teflon resin is less than that of Hastelloy and the molten Teflon resin, the main part is processed by the method of the present invention to extrude the Teflon-coated wire. The lubricity of the lower surface is good, and the extruded coated wire has the advantage of smooth surface.

상술한 바와 같이 본 발명에 의하면, 금속표면에 ΑlＦ3, Al(ＦχＯy)n등의 불소화합물을 포함하는 다층 이온도금 처리하여 불소가스 분위기 하에서의 절삭공구나 금속 부품의 산화방지를 가능하게 하여, 종래보다 경도가 높고 내마모성이 우수하며 고속절삭 공구의 수명을 수배로 증진시킬 수 있는 특장점을 갖는다.As described above, according to the present invention, a multi-layer ion plating treatment containing fluorine compounds such as AlF 3 and Al (F x O y ) n on the metal surface enables oxidation prevention of cutting tools or metal parts in a fluorine gas atmosphere. Thus, it has a feature that the hardness is higher than the conventional, excellent wear resistance, and can increase the life of the high speed cutting tool several times.

Claims (2)

절삭공구 또는 HF 가스에 노출되는 금속표면에 PEPVD 혹은 PECVD 방법으로 TiAlN을 이온 도금한 후 200∼400℃의 대기중에 1∼3시간동안 노출시켜 도금층 표면에 Al2O3층을 형성시킨 후 350∼400℃의 HF 가스 분위기 하에 1∼6시간 동안 노출시켜 도금층 표면에 AlF3나 Al(ＦχＯy)n층을 형성시키는 것을 특징으로 하는 금속표면에 불소화합물을 포함하는 다층 이온도금 방법.TiAlN was ion-plated on the metal surface exposed to the cutting tool or HF gas, and then exposed for 1 to 3 hours in the atmosphere at 200 to 400 ° C to form an Al 2 O 3 layer on the surface of the plating layer. A multi-layer ion plating method comprising a fluorine compound on a metal surface, wherein an AlF 3 or Al (F x O y ) n layer is formed on the surface of the plating layer by exposing for 1 to 6 hours in an HF gas atmosphere at 400 ° C. 제 1항에 있어서, 상기 TiAlN을 이온 도금한 후 350∼400℃의 공기와 HF 가스의 혼합하에 1∼6시간동안 노출시켜 TiAlN 도금층 표면에 ΑlＦ3나 Al(ＦχＯy)n층을 형성시키는 것을 특징으로 하는 금속표면에 불소화합물을 포함하는 다층 이온도금 방법.The AlF 3 or Al (F x O y ) n layer is formed on the surface of the TiAlN plated layer by exposing the TiAlN to ion plating and exposing it for 1 to 6 hours under a mixture of 350 to 400 ° C. air and HF gas. A multi-layer ion plating method comprising a fluorine compound on the metal surface, characterized in that.
KR1019990039700A 1999-09-15 1999-09-15 Multilayer ion-coating method being fluorine compound on metal surface KR100321613B1 (en)

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