KR20000046427A - Method for preparing diamond-form carbon film - Google Patents

Method for preparing diamond-form carbon film Download PDF

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Publication number
KR20000046427A
KR20000046427A KR1019980063107A KR19980063107A KR20000046427A KR 20000046427 A KR20000046427 A KR 20000046427A KR 1019980063107 A KR1019980063107 A KR 1019980063107A KR 19980063107 A KR19980063107 A KR 19980063107A KR 20000046427 A KR20000046427 A KR 20000046427A
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diamond
carbon film
intermediate layer
layer
composition
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KR1019980063107A
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Korean (ko)
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송근철
최준엽
전영찬
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추호석
대우중공업 주식회사
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Priority to KR1019980063107A priority Critical patent/KR20000046427A/en
Publication of KR20000046427A publication Critical patent/KR20000046427A/en

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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B9/00—Layered products comprising a layer of a particular substance not covered by groups B32B11/00 - B32B29/00
    • B32B9/005—Layered products comprising a layer of a particular substance not covered by groups B32B11/00 - B32B29/00 comprising one layer of ceramic material, e.g. porcelain, ceramic tile
    • B32B9/007—Layered products comprising a layer of a particular substance not covered by groups B32B11/00 - B32B29/00 comprising one layer of ceramic material, e.g. porcelain, ceramic tile comprising carbon, e.g. graphite, composite carbon
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B7/00—Layered products characterised by the relation between layers; Layered products characterised by the relative orientation of features between layers, or by the relative values of a measurable parameter between layers, i.e. products comprising layers having different physical, chemical or physicochemical properties; Layered products characterised by the interconnection of layers
    • B32B7/04—Interconnection of layers
    • B32B7/12—Interconnection of layers using interposed adhesives or interposed materials with bonding properties
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B9/00—Layered products comprising a layer of a particular substance not covered by groups B32B11/00 - B32B29/00
    • B32B9/04—Layered products comprising a layer of a particular substance not covered by groups B32B11/00 - B32B29/00 comprising such particular substance as the main or only constituent of a layer, which is next to another layer of the same or of a different material
    • B32B9/041—Layered products comprising a layer of a particular substance not covered by groups B32B11/00 - B32B29/00 comprising such particular substance as the main or only constituent of a layer, which is next to another layer of the same or of a different material of metal

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  • Engineering & Computer Science (AREA)
  • Ceramic Engineering (AREA)
  • Chemical & Material Sciences (AREA)
  • Crystals, And After-Treatments Of Crystals (AREA)
  • Chemical Vapour Deposition (AREA)

Abstract

PURPOSE: A method for preparing a diamond-form carbon film is provided to improve the adhesion of the carbon film to an intermediate layer formed between a metal parent material and diamond-form carbon film. CONSTITUTION: A method for preparing a diamond-form carbon film according to the present invention comprises forming an intermediate layer between a metal parent material and the diamond-form carbon film and is characterized in that the method comprises forming a composition-gradient layer having gradient of composition ranged from the composition of intermediate layer to the composition of diamond-form carbon film between the intermediate layer and diamond-form carbon film.

Description

다이아몬드상 카본 필름의 제조방법(Method of manufacturing carbon film with diamond phase)Method of manufacturing carbon film with diamond phase

본 발명은 다이아몬드상 카본필름의 제조방법에 관한 것으로, 특히 우수한 내마모성과 윤활성, 내약품성, 내식성 등을 가지면서도 금속계 모재에 대한 접착력을 향상시킬 수 있는 다이아몬드상 카본필름의 제조방법에 관한 것이다.The present invention relates to a method for producing a diamond-like carbon film, and more particularly to a method for producing a diamond-like carbon film that can improve the adhesion to a metallic base material while having excellent wear resistance, lubricity, chemical resistance, corrosion resistance and the like.

일반적으로 다이아몬드상 카본필름은 우수한 마찰특성, 마모특성, 열전도성 및 내식성을 갖는 물질로, 도 1에 도시된 바와 같이 금속계 모재(10)의 표면에 PECVD, 스퍼터링, 이온플레이팅, ECR, 레이저 어블레이션, 플라즈마 등의 다양한 증착방법으로 다이아몬드상 카본필름층(12)을 형성시켜 내마모성, 윤활성, 내약품성, 내식성 등이 요구되는 부품에 사용되고 있으나, 다이아몬드상 카본필름과 금속계의 모재는 상호 접착력이 좋지 않은 문제가 있어 박리가 쉽게 일어나게 되는 문제점이 있다.In general, diamond-like carbon film is a material having excellent friction properties, wear characteristics, thermal conductivity and corrosion resistance, PECVD, sputtering, ion plating, ECR, laser ablation on the surface of the metal base material 10 as shown in FIG. The diamond-like carbon film layer 12 is formed by various deposition methods such as ration and plasma, and is used in parts requiring wear resistance, lubricity, chemical resistance, and corrosion resistance, but the diamond-like carbon film and the metal base metal have good mutual adhesion. There is a problem that does not have a problem that peeling easily occurs.

그래서 이러한 문제를 해결하기 위하여 도 2에 도시된 바와 같이, 금속계 모재(10)의 표면에 소정의 중간층(14)을 증착시킨 후, 이 중간층(14)위에 다시 다이아몬드상 카본필름층(12)을 증착시키므로써, 즉 금속계모재(10)와 다이아몬드상 카본필름층(12) 사이에 금속계 모재 및 다이아몬드상 카본필름 모두에 대하여 우수한 접착성능을 가지는 재료로 중간층(14)을 형성하여 우수한 접착 특성을 얻을 수 있게 되는 것이다.Therefore, in order to solve this problem, as shown in FIG. 2, after depositing a predetermined intermediate layer 14 on the surface of the metallic base 10, the diamond-like carbon film layer 12 is again deposited on the intermediate layer 14. By depositing, that is, the intermediate layer 14 is formed of a material having excellent adhesion to both the metallic base material and the diamond-like carbon film between the metallic base material 10 and the diamond-like carbon film layer 12 to obtain excellent adhesion characteristics. It will be possible.

이와같이 금속계 모재(10)와 상기 다이아몬드상 카본필름층(12)의 사이에 상기 중간층(14)을 증착시키는 방법에 의해서 종래의 다이아몬드상 카본필름으로 금속계 모재(10)에 직접 증착하는 것이 용이하지 않은 경우에도 다이아몬드상 카본필름의 증착할 수 있게 되었다.As described above, the intermediate layer 14 is deposited between the metallic base 10 and the diamond-like carbon film layer 12, and thus it is not easy to directly deposit the metallic base 10 with the conventional diamond-like carbon film. Even in the case of diamond-like carbon film can be deposited.

이러한 방법에 따라 현재 다양한 형태의 중간층이 도입되고 있는 바, 이러한 중간층을 도입하므로써 금속기지에 대해서도 다이아몬드 카본필름이 증착하는 것이 가능해졌으나, 중간층과 다이아몬드상 카본필름사이에 또다시 새로운 계면이 생성되므로써 다이아몬드상 카본필름에 높은 하중이나 충격이 가해지는 경우 이 부분으로 부터 쉽게 박리가 일어나는 문제들이 발생하였다.According to this method, various types of intermediate layers are currently introduced. By introducing such intermediate layers, diamond carbon films can be deposited on metal bases, but diamonds are formed by creating new interfaces between the intermediate layers and the diamond-like carbon films. When high loads or impacts are applied to the upper carbon film, problems arise in that peeling easily occurs from this part.

도 3은 침탄열처리한 강재에 다이아몬드상 카본필름을 증착하여 제작한 시편에 압입자가 다이아몬드콘인 록크웰경도기로 압흔을 만들어 압흔주위의 필름 탈락형태를 관찰한 사진을 나타낸 것으로, 이 사진에서 알 수 있는 바와 같이 다이아몬드상 카본필름층(12)과 중간층(14) 사이에서 박리가 일어났음을 알 수 있다.FIG. 3 is a photograph showing the indentation of the diamond-like carbon film on the carburized heat-treated steel to make an indentation using a Rockwell hardness tester, a diamond cone, to observe the film dropout form around the indentation. As can be seen, peeling occurred between the diamond-like carbon film layer 12 and the intermediate layer 14.

따라서 전체적인 다이아몬드상 카본필름의 접착강도를 높이기 위해서는 중간층과 다이아몬드상 카본필름 사이의 계면에서의 접착력이 가장 중요한 관건이 되어 왔다.Therefore, in order to increase the adhesive strength of the overall diamond-like carbon film, the adhesion at the interface between the intermediate layer and the diamond-like carbon film has been the most important.

이에 본 발명은 상기한 문제점을 해결하기 위한 것으로, 금속모재와 다이아몬드상 카본필름 사이에 형성된 중간층과 다이아몬드상 카본필름간의 접착력을 향상시키는 다이아몬드상 카본필름의 제조방법을 제공하는 데 그 목적이 있다.Accordingly, an object of the present invention is to provide a method of manufacturing a diamond-like carbon film that improves the adhesion between the diamond-like carbon film and the intermediate layer formed between the metal base material and the diamond-like carbon film.

상기한 목적을 달성하기 위한 본 발명의 다이아몬드상 카본필름의 제조방법은, 중간층을 이루는 물질과 다이아몬드상 카본필름 사이에 중간층으로 부터 다이아몬드상 카본필름 조성으로 점차 변화해가도록 조성의 구배를 준 조성구배층을 형성하게 된 것을 특징으로 한다.In the method for producing a diamond-like carbon film of the present invention for achieving the above object, a composition gradient giving a gradient of composition so as to gradually change from the intermediate layer to the diamond-like carbon film composition between the material forming the intermediate layer and the diamond-like carbon film. Characterized in that it forms a layer.

상기한 본 발명에 따르면, 중간층과 다이아몬드상 카본필름 간에 조성구배층을 형성하므로써 중간층과 다이아몬드상 카본필름 층사이에 계면이 형성되지 않도록 하여 계면에서 일어나는 박리현상을 근본적으로 억제하는 효과가 있다.According to the present invention described above, by forming a composition gradient layer between the intermediate layer and the diamond-like carbon film, there is an effect of fundamentally suppressing the peeling phenomenon occurring at the interface by preventing the interface between the intermediate layer and the diamond-like carbon film layer.

도 1은 다이아몬드상 카본필름을 직접 증착된 금속모재의 단면도,1 is a cross-sectional view of a metal base material directly deposited diamond-like carbon film,

도 2는 다이아몬드상 카본필름이 중간층을 매개로 증착된 금속모재의 단면도,2 is a cross-sectional view of a metal base material on which a diamond-like carbon film is deposited through an intermediate layer;

도 3은 종래방법에 따라 다이아몬드상 카본필름이 증착된 시편의 압흔을 나타낸 사진,Figure 3 is a photograph showing the indentation of the specimen is deposited diamond-like carbon film according to the conventional method,

도 4은 본 발명에 따른 다이아몬드상 카본필림의 증착된 금속모재의 개략적인 단면도이다.4 is a schematic cross-sectional view of the deposited metal base material of the diamond-like carbon film according to the present invention.

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

10 : 금속계 모재 12 : 다이아몬드상 카본필름10 metal base material 12 diamond-like carbon film

14 : 중간층 16 : 조성구배층14: intermediate layer 16: composition gradient layer

이하, 첨부된 도면을 참조하여 본 발명의 실시예를 상세하게 설명하면 다음과 같다.Hereinafter, exemplary embodiments of the present invention will be described in detail with reference to the accompanying drawings.

도 4는 본 발명에 따라 다이아몬드상 카본필름을 증착시킨 금속계모재의 단면을 도시한 도면으로, 금속계모재(10)의 상부에 금속계 모재와 접착력이 우수한 재질의 중간층(14)을 증착시키고, 이 중간층(14)위에 다시 중간층을 이루는 원료가스와 다이아몬드상 카본필름을 증착시키는 원료가스를 혼합하여 조성이 중간층에서 다이아몬드카본필름으로 점차적으로 구배를 이루도록 된 조성구배층(16)을 형성하고, 이 조성구배층(16)위에 다이아몬드상 카본필름을 증착시키는 원료가스만을 공급하여 다이아몬드상 카본필름층(12)을 증착한 구조로 되어 있다.4 is a cross-sectional view of a metal-based base material on which a diamond-like carbon film is deposited according to the present invention. The intermediate layer 14 of a material having excellent adhesion with the metal-based base material is deposited on the metal-based base material 10, and the intermediate layer is deposited. (14) forming a composition gradient layer 16 in which a composition gas gradually forms a gradient from the intermediate layer to the diamond carbon film by mixing the source gas forming the intermediate layer and the source gas for depositing the diamond-like carbon film again. Only the raw material gas for depositing the diamond-like carbon film on the layer 16 is supplied, and the diamond-like carbon film layer 12 is deposited.

여기서 상기 중간층을 비정질규소로 증착한 경우, 종래에는 비정질규소의 원료가스의 공급을 단절한 후 다이아몬드상 카본의 원료가스를 공급하여 필름을 증착하는 단계이전에 중간층을 형성하는 원료가스와 다이아몬드상 카본필름을 증착시키는 원료가스를 혼합시켜 증착하는 단계를 삽입하므로써 중간층과 다이아몬드상 카본의 혼합영역을 형성하도록 한다.Here, when the intermediate layer is deposited with amorphous silicon, the source gas and the diamond-like carbon which form the intermediate layer before the step of depositing a film by supplying the source gas of diamond-like carbon after supplying the source gas of amorphous silicon, conventionally By inserting a deposition step of mixing the source gas for depositing the film to form a mixed region of the intermediate layer and the diamond-like carbon.

이하에서 CVD법에 의한 증착방법을 사용하는 경우에 있어서 본 발명에 따라 다이아몬드상 카본필름을 형성하는 과정을 단계별로 상세히 살펴보면, 금속모재 표면에 비정질 규소층을 증착시키는 중간층 증착단계와, 챔버에 다이아몬드상 카본의 원료가스를 투입하기 시작함과 아울러 상기 중간층의 원료가스양을 점차 줄여주어 다이아몬드상 카본의 원료가스 양을 늘려가는 조성구배층을 증착하는 조성구배층 증착단계 및, 중간층 원료가스의 투입을 중단하고 다이아몬드상 카본의 원료가스만을 투입하여 순수한 다이아몬드상 카본필름을 증착하는 단계로 구성된다.Hereinafter, a detailed step-by-step process of forming a diamond-like carbon film according to the present invention in the case of using a deposition method by CVD method, an intermediate layer deposition step of depositing an amorphous silicon layer on the surface of the metal base material, and diamond in the chamber A composition gradient layer deposition step of depositing a composition gradient layer for increasing the amount of source gas of diamond-like carbon by gradually reducing the amount of source gas of the intermediate layer by gradually inputting the source gas of phase carbon, and inputting the intermediate layer source gas It stops and consists of depositing pure diamond-like carbon film by inputting only raw material gas of diamond-like carbon.

이와같은 단계로 다이아몬드상 카본필름을 증착하므로써 다이아몬드상 카본필름이 금속모재에 대한 우수한 접착력을 가질 수 있게 된다.By depositing the diamond-like carbon film in this step, the diamond-like carbon film can have excellent adhesion to the metal base material.

[실시예]EXAMPLE

경질크롬도금한 금속모재상에 비정질 탄화규소를 중간층으로 형성시키고 그위에 메탄가스를 선구물질로 하는 다이아몬드상 카본필름을 PECVD방법을 이용하여 증착하였다.An amorphous silicon carbide was formed as an intermediate layer on the hard chromium-plated metal base material, and a diamond-like carbon film containing methane as a precursor was deposited by PECVD.

이때 증간층의 원료가스로는 SiH4/H2혼합가스와 메탄가스를 사용하여, 비정질 탄화규소층을 800nm정도 금속모재의 크롬도금층위에 중간층을 증착하여 형성하였다.At this time, as the raw material gas of the thick layer, SiH 4 / H 2 mixed gas and methane gas were used, and an amorphous silicon carbide layer was formed by depositing an intermediate layer on a chromium plated layer of a metal base material about 800 nm.

그리고, SiH4/H2혼합가스와 메탄가스의 비를 연속적으로 변화시켜 약 200nm 두께의 농도구배층을 형성시킨 후, 마지막으로 메탄가스만을 사용하여 순수한 다이아몬드상 카본필름을 약 4000nm 두께로 증착하였다.Then, the ratio of SiH 4 / H 2 mixed gas and methane gas was continuously changed to form a concentration gradient layer having a thickness of about 200 nm, and finally pure diamond-like carbon film was deposited to about 4000 nm thickness using only methane gas. .

상기한 조건으로 마모시험편을 제작하고, 동일한 조성으로 농도구배층 없이 1000nm 두께의 중간층 위에 직접 4000nm두께의 다이아몬드상 카본필름을 증착한 시편을 제작하여 마모시험을 통해 두 공정으로 제작한 시편 간의 필름의 접착력을 비교하였다.Abrasion test specimens were prepared under the above conditions, and a specimen was fabricated by depositing a diamond-like carbon film of 4000 nm thickness directly on a 1000 nm-thick intermediate layer without a concentration gradient layer with the same composition. Adhesion was compared.

이와 같은 두종류의 시험편에 대하여 마모시험을 행한 결과 조성의 구배를 주어 중간층과 다이아몬드상 카본필름 사이에 계면이 형성되지 않은 경우 약 30시간만에 필름의 박리가 발생하였으나, 조성구배를 주지 않은 시편의 경우 13시간만에 필름의 박리가 발생하였다.As a result of the abrasion test of these two types of specimens, when the interface was not formed between the intermediate layer and the diamond-like carbon film, the film peeled in about 30 hours, but the composition was not given the gradient. In the case of peeling of the film occurred in 13 hours.

이상에서 살펴본 바와 같이, 본 발명은 중간층과 다이아몬드상 카본필름층사이에 조성구배층을 개재시키므로써 다이아몬드상 카본필름의 접착력을 향상시키는 효과가 있다.As described above, the present invention has the effect of improving the adhesion of the diamond-like carbon film by interposing a composition gradient layer between the intermediate layer and the diamond-like carbon film layer.

Claims (1)

금속모재와 다이아몬드상 카본필름 사이에 중간층을 형성하게 된 다이아몬드상 카본필름의 제조방법에 있어서, 상기 중간층과 상기 다이아몬드상 카본필름 사이에 중간층의 조성과 다이아몬드상 카본필름의 조성간에 조성의 구배를 가지는 조성구배층을 형성하게 된 것을 특징으로 하는 다이아몬드상 카본필름의 제조방법.A method for producing a diamond-like carbon film in which an intermediate layer is formed between a metal base material and a diamond-like carbon film, wherein the composition has a gradient between the composition of the intermediate layer and the composition of the diamond-like carbon film between the intermediate layer and the diamond-like carbon film. Method for producing a diamond-like carbon film, characterized in that to form a composition gradient layer.
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KR100779303B1 (en) * 2007-02-07 2007-11-23 두산인프라코어 주식회사 Method for coating diamond-like carbon film on hydraulic generator piston
KR101470320B1 (en) * 2013-01-17 2014-12-08 연세대학교 산학협력단 Functional coating structure for wear and friction reduction and method thereof
KR20150076468A (en) * 2013-12-26 2015-07-07 재단법인 포항산업과학연구원 Nitride coating layer and the method thereof

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US5629086A (en) * 1993-07-07 1997-05-13 Sanyo Electric Co., Ltd. Hard-carbon-film-coated substrate and apparatus for forming the same
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KR920004081A (en) * 1990-08-04 1992-03-27 야마모도 다꾸마 Vapor deposition method of diamond film and its apparatus
US5629086A (en) * 1993-07-07 1997-05-13 Sanyo Electric Co., Ltd. Hard-carbon-film-coated substrate and apparatus for forming the same
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* Cited by examiner, † Cited by third party
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KR100779303B1 (en) * 2007-02-07 2007-11-23 두산인프라코어 주식회사 Method for coating diamond-like carbon film on hydraulic generator piston
KR101470320B1 (en) * 2013-01-17 2014-12-08 연세대학교 산학협력단 Functional coating structure for wear and friction reduction and method thereof
KR20150076468A (en) * 2013-12-26 2015-07-07 재단법인 포항산업과학연구원 Nitride coating layer and the method thereof

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