KR20040035528A - Coloring of titanium using ion implantation - Google Patents

Coloring of titanium using ion implantation Download PDF

Info

Publication number
KR20040035528A
KR20040035528A KR1020020064703A KR20020064703A KR20040035528A KR 20040035528 A KR20040035528 A KR 20040035528A KR 1020020064703 A KR1020020064703 A KR 1020020064703A KR 20020064703 A KR20020064703 A KR 20020064703A KR 20040035528 A KR20040035528 A KR 20040035528A
Authority
KR
South Korea
Prior art keywords
titanium
oxide film
coloring
ion implantation
heat treatment
Prior art date
Application number
KR1020020064703A
Other languages
Korean (ko)
Inventor
송오성
이정임
홍석배
Original Assignee
송오성
이정임
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by 송오성, 이정임 filed Critical 송오성
Priority to KR1020020064703A priority Critical patent/KR20040035528A/en
Publication of KR20040035528A publication Critical patent/KR20040035528A/en

Links

Classifications

    • 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
    • C23C8/36—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 using ionised gases, e.g. ionitriding
    • 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
    • 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
    • C23C8/24—Nitriding
    • 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
    • C23C8/80—After-treatment

Landscapes

  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Physical Vapour Deposition (AREA)

Abstract

PURPOSE: A method for coloring titanium by ion implantation is provided to obtain more various colors compared to existing colors and improve hardness of the surface by adding ion implantation and heat treatment processes to titanium coloring process. CONSTITUTION: The method for coloring titanium by ion implantation comprises the steps of forming a titanium oxide film on the surface of titanium metal by thermal oxidation or wet oxidation; ion injecting an arbitrary material for coloring a certain color into the titanium oxide film so that specific colors are improved and changed into other colors; and performing heat treatment process as occasion demands, wherein the arbitrary material comprises N, O, B and transition metal ions, wherein the titanium oxide film comprises oxide film, nitride film and membrane for obtaining discoloring effect by surface pitting to color the surface of the titanium oxide film, and wherein the heat treatment process for improving surface strength is performed by using existing electric furnace and rapid heating method.

Description

이온주입에 의한 티타늄 발색 {Coloring of titanium using ion implantation}Coloring of titanium using ion implantation

Ti와 그의 합금 표면에 산화막을 생성시켜 이 막에 의한 발색효과로 미려한 표면을 얻는 기술은 의장용 목적 및 건축자재, 생활용품 등의 심미적 목적으로 개발되어 왔다.A technique of forming an oxide film on the surface of Ti and its alloy and obtaining a beautiful surface by the color development effect of the film has been developed for aesthetic purposes such as design purposes, building materials, and household goods.

표면의 발색은 산화막의 두께와 치밀도에 따른 결함밀도에 크게 영향 받으므로 일단 목적하는 두께의 티타늄 산화막을 생성시키기 위해서 이제까지 건식법, 아노다이징 방법의 습식법이 주로 사용되었고 그 외 TiN등의 질화물로써 진회색의 코팅을 하는 방법과 표면부식에 의한 회색(흑색)화 기술이 적용되었으나 각각 장단점이 있다.The color development of the surface is greatly influenced by the defect density according to the thickness and density of the oxide film. Therefore, the wet method of the dry method and the anodizing method has been mainly used to produce the titanium oxide film of the desired thickness. The method of coating and graying by surface corrosion has been applied, but each has its advantages and disadvantages.

건식식각법은 목표하는 온도에 산소분위기하에서 열처리하여 표면에 균일한 열산화막을 생성하는 방법으로, 많은 양의 티타늄 요소를 한번에 처리하는 것이 가능하지만 형상에 따른 온도구배 차이에 의한 발색효과가 불균일하게 생길 수 있는 단점이 있다.Dry etching is a method of producing a uniform thermal oxide film on the surface by heat treatment under the oxygen atmosphere at the target temperature, and it is possible to treat a large amount of titanium element at once, but the coloring effect due to the temperature gradient difference according to the shape is uneven. There are disadvantages that can occur.

습식법은 비교적 간단히 표면부를 (+)로하여 전해액하에서 전류를 가하여 양극 산화시키는 것으로 쉽게 선형적인 두께 변화를 예측하여 여러 가지 발색이 가능하지만 고전압에서 생기는 녹색, 적색 발색을 위해서는 과전류 발생에 따른 유해가스 발생 등의 단점이 있다.In the wet method, it is relatively simple to make anodization by applying a current under an electrolyte by making the surface part (+) relatively easy to predict linear thickness change, and various colors are possible. There are disadvantages.

TiN등의 질화물을 만드는 방법은 주로 흑색 계열의 발색을 위해서 사용되지만 1500 ℃ 의 고온반응로가 필요하고 여러 가지 색의 발색이 불가능한 단점이 있다.The method of making nitrides such as TiN is mainly used for black color development, but requires a high temperature reaction furnace of 1500 ° C., and it is impossible to develop various colors.

간단히 불산 및 황산등의 혼합수용액에 침지시켜 표면을 일정량 부식시켜 무광택의 티타늄 표면을 얻는 흑색화 작업은 용접부가 드러나거나 다양한 발색효과는 없는 단점이 있었다.The blackening operation to obtain a matt titanium surface by simply immersing in a mixed solution such as hydrofluoric acid and sulfuric acid to corrode a certain amount of the surface has a disadvantage in that the welded part is exposed or there are no various coloring effects.

따라서 본 발명은 상기 문제중 다양한 색채의 구현이 어려운 단점을 특정 산화막을 생성시키고 이때 발생하는 색을 결정하고, 이 산화막 표면에 선택적으로 N+, O-, B+ 등 특정 이온을 이온주입하여 새로운 색의 발색이 가능하도록 하는 방법에 관한 것이다.Therefore, in the present invention, it is difficult to implement various colors among the above problems. A specific oxide film is generated, and a color generated at this time is determined. The present invention relates to a method for enabling color development.

따라서, 본 발명은 상기와 같은 종래의 제한된 티타늄 발색범위 문제점을 고려하여 안출한 것으로써, 그 목적은 티타늄 발색공정에 이온주입과 열처리공정을 부가하여 기존의 색보다 다양한 색과 표면경도를 향상시킬 수 있는 기능성을 갖게하는데 있다.Therefore, the present invention has been made in view of the problems of the conventional limited titanium color range as described above, the object is to add ion implantation and heat treatment process to the titanium color development process to improve a variety of colors and surface hardness than conventional colors It is to have the functionality that can be.

도 1은 본 발명에 따른 티타늄의 발색가공공정을 예시하는 개략도.1 is a schematic diagram illustrating a color processing process of titanium according to the present invention.

도 2는 본 발명에 따른 티타늄시료의 표면경도 결과 그래프.Figure 2 is a graph of the surface hardness of the titanium sample according to the present invention.

상기 목표를 이루기 위해 실시 예로서 2 ㎛의 두꺼운 열산화 TiO2표면부에 70 keV로 dose 1017ions/㎠ 조건의 N+ 이온주입을 실시한 경우를 상정한 공정을 표시한다.In order to achieve the above object, a process assuming a case where N + ion implantation is performed at a dose of 10 17 ions / cm 2 at 70 keV at a surface portion of 2 μm thick thermally oxidized TiO 2 is shown.

[도1]에 제안한 발명의 공정도를 나타내었다.1 shows a process diagram of the proposed invention.

첫째는 준비된 티타늄 시료를 975 ℃ - 30 min 조건으로 대기 중 조건하에서 열산화막을 형성시켜 소정 색을 갖게 한다. 실시예로서 본 발명에서는 직경 10 mm, 두께 1mm의 동전형 티타늄 시편 전면에 하얀색의 산화막이 생성되었다. 물론 목적에 맞게 열산화막 형성 온도와 시간을 조절하여 노란색, 파란색 등 필요에 맞는 소정 색의 구현은 가능하다.First, the prepared titanium sample is formed at a temperature of 975 ° C.-30 min under a thermal oxide film to have a predetermined color. As an example, in the present invention, a white oxide film was formed on the entire surface of a coin-shaped titanium specimen having a diameter of 10 mm and a thickness of 1 mm. Of course, by adjusting the temperature and time of forming the thermal oxide film according to the purpose, it is possible to implement a predetermined color to meet the needs, such as yellow, blue.

두 번째 공정으로, 이미 발색된 시편의 전면 또는 특정부에 소정이온의 이온주입을 실시한다. 실시예로서 본 발명에서는 70 keV 의 에너지로 이온의 양을 dose 2, 5, 10x1016ions/㎠ 조건으로 N+ 이온주입을 실시하였다. 이러한 이온주입에 의해 최종적으로 흰색에서 이온주입 양의 증가에 따라 갈색으로 변화가 가능하였다.In the second process, ion implantation of predetermined ions is performed on the front surface or a specific portion of the already developed specimen. As an example, in the present invention, N + ion implantation was performed under conditions of dose 2, 5, and 10 × 10 16 ions / cm 2 with an energy of 70 keV. By the ion implantation, it was finally possible to change from white to brown as the amount of ion implantation increased.

세 번째 부가공정으로, 필요에 따라 열처리공정을 더 할 수 있다. 본 발명에서는 실시예로서 산소와의 접촉에 따른 산화막의 증가에 의한 색변화를 방지하고자 Ar불활성 가스 분위기와 진공분위기에서 600 ℃ - 120 min 조건으로 열처리를 진행하였다.As a third additional step, a heat treatment step may be added as necessary. In the present invention, in order to prevent the color change by the increase of the oxide film in accordance with the contact with oxygen, the heat treatment was performed at 600 ℃-120 min conditions in an Ar inert gas atmosphere and a vacuum atmosphere.

결과적으로 열처리와 이온주입에 따라 [도2]와 같이 표면경도의 변화가 발생하였고, 제품특성상 내구성을 높이기 위해서는 이온주입과 열처리공정을 부가하면 가능하였다.As a result, a change in surface hardness occurred as shown in [2] according to heat treatment and ion implantation, and it was possible to add ion implantation and heat treatment processes in order to increase durability in product characteristics.

기존 티타늄 및 그의 합금제품의 표면발색 기술 중 이온주입 공정과 열처리공정을 부가하여 새론운 색상을 발색하고 경우에 따라서는 표면경도를 향상시켜 내구성을 증가시킬 수 있는 기술로서, 장신구 및 생활용품으로 채용되면 심미적인 효과와 내구성을 강화한 제품이 가능하다.It is a technology that can develop new color by adding ion implantation process and heat treatment process among surface color development technology of existing titanium and its alloy products, and sometimes increase durability by improving surface hardness. When aesthetic effects and durable products are available.

Claims (4)

임의의 티타늄 금속표면에 열산화 또는 습식산화에 의해 티타늄 산화막을 형성시키고 이 산화층에 특정색을 내게되는 임의 물질을 이온주입하여 특정한 색의 향상 또는 다른색으로 변색시키는 기술과 필요에 따라 열처리를 부가하여 표면강도를 향상시키는 기술.Titanium oxide film is formed on any titanium metal surface by thermal oxidation or wet oxidation, and any material giving a specific color to the oxide layer is ion-implanted to improve specific color or discolor to another color, and to add heat treatment as necessary. Technology to improve the surface strength. 상기 1항의 임의물질은 N, O, B와 천이금속 이온을 포함함을 특징으로 한다.The optional substance of claim 1 is characterized in that it comprises N, O, B and transition metal ions. 상기 1항의 타타늄 산화막은 표면 발색을 위한 것이므로 산화막, 질화막, 표면 pit 등에 의한 변색 효과를 주는 막질을 포함함을 특징으로 한다.Since the titanium oxide film of claim 1 is for surface color development, it is characterized in that it comprises a film having a discoloring effect by an oxide film, a nitride film, a surface pit, and the like. 상기 1항의 열처리를 부가하여 표면강도를 향상시키는 공정은 기존의 전기로 및 급속가열 방식을 포함함을 특징으로 한다.The process of improving the surface strength by adding the heat treatment of claim 1 is characterized in that it comprises a conventional electric furnace and rapid heating method.
KR1020020064703A 2002-10-22 2002-10-22 Coloring of titanium using ion implantation KR20040035528A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
KR1020020064703A KR20040035528A (en) 2002-10-22 2002-10-22 Coloring of titanium using ion implantation

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
KR1020020064703A KR20040035528A (en) 2002-10-22 2002-10-22 Coloring of titanium using ion implantation

Publications (1)

Publication Number Publication Date
KR20040035528A true KR20040035528A (en) 2004-04-29

Family

ID=37334445

Family Applications (1)

Application Number Title Priority Date Filing Date
KR1020020064703A KR20040035528A (en) 2002-10-22 2002-10-22 Coloring of titanium using ion implantation

Country Status (1)

Country Link
KR (1) KR20040035528A (en)

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR20040035530A (en) * 2002-10-22 2004-04-29 송오성 Titanium coloring with top-down selective etching
KR20190122463A (en) * 2018-04-20 2019-10-30 한국과학기술연구원 Ion-implanted coloring alloy and method for preparing thereof

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS63118061A (en) * 1986-11-07 1988-05-23 Toobi:Kk Production of hard colored oxide film
JPH01108360A (en) * 1987-10-20 1989-04-25 Seiko Instr & Electron Ltd Outer ornament parts for watch
JPH02149663A (en) * 1988-11-30 1990-06-08 Hitachi Ltd Formation of titanium nitride film by dynamic mixing
JPH0499870A (en) * 1990-08-16 1992-03-31 Nisshin Steel Co Ltd Production of ceramic coating material
KR0166665B1 (en) * 1996-01-31 1999-01-15 김희용 Colouring method for decorating a metal surface by ion beam coating

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS63118061A (en) * 1986-11-07 1988-05-23 Toobi:Kk Production of hard colored oxide film
JPH01108360A (en) * 1987-10-20 1989-04-25 Seiko Instr & Electron Ltd Outer ornament parts for watch
JPH02149663A (en) * 1988-11-30 1990-06-08 Hitachi Ltd Formation of titanium nitride film by dynamic mixing
JPH0499870A (en) * 1990-08-16 1992-03-31 Nisshin Steel Co Ltd Production of ceramic coating material
KR0166665B1 (en) * 1996-01-31 1999-01-15 김희용 Colouring method for decorating a metal surface by ion beam coating

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR20040035530A (en) * 2002-10-22 2004-04-29 송오성 Titanium coloring with top-down selective etching
KR20190122463A (en) * 2018-04-20 2019-10-30 한국과학기술연구원 Ion-implanted coloring alloy and method for preparing thereof

Similar Documents

Publication Publication Date Title
TW201402865A (en) Surface treatment method for metal substrate and article manufactured by the same
Guzman et al. Ion beam induced enhanced adhesion of Au films deposited on polytetrafluoroethylene
KR20040035528A (en) Coloring of titanium using ion implantation
KR940001677B1 (en) Sputtering apparatus
DE60235071D1 (en) Iron
US4518467A (en) Selective solar surfaces
KR20180070099A (en) Metal spacer for camera lens and manufacuring method thereof
JPS6213563A (en) Method for coloring stainless steel
KR20180106046A (en) Copper plating metal spacer for camera lens and manufacuring method thereof
KR860007722A (en) Improved insulating film processing method and wafer and integrated circuit manufactured according to the processing method
KR910003037B1 (en) Oxide color treatment for a stainless steel
RU2081947C1 (en) Method for manufacturing coating
JPH0499870A (en) Production of ceramic coating material
JPH02294467A (en) Method for coloring surface of metallic material and product obtained by it
JPS58221283A (en) Pretreatment of stainless steel before coloring
RU2618283C1 (en) Method of image application on precious metals products
JPH05156425A (en) Ornamental member and its production
JPH06330349A (en) Colored ti plated material
JPS6134171A (en) Production of catalytic material
CN201132817Y (en) Golden yellow coated glass or ceramic
KR100834183B1 (en) Method for manufacturing color material having oxide layer with high corrosion-resistance be formed design
JPH0339498A (en) High corrosion resistant chromium plating stainless steel product and production thereof
JPS63199894A (en) Method for electrolytically developing color on titanium and titanium alloy
JPS61219607A (en) Mold for plastic
CN107109665A (en) Clock and watch screw and its manufacture method

Legal Events

Date Code Title Description
A201 Request for examination
E902 Notification of reason for refusal
E601 Decision to refuse application