KR20040023447A - Coloring of Jewelry Stones using Ion implantation and Annealing - Google Patents
Coloring of Jewelry Stones using Ion implantation and Annealing Download PDFInfo
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- KR20040023447A KR20040023447A KR1020020055177A KR20020055177A KR20040023447A KR 20040023447 A KR20040023447 A KR 20040023447A KR 1020020055177 A KR1020020055177 A KR 1020020055177A KR 20020055177 A KR20020055177 A KR 20020055177A KR 20040023447 A KR20040023447 A KR 20040023447A
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- 238000005468 ion implantation Methods 0.000 title claims description 28
- 238000004040 coloring Methods 0.000 title description 6
- 239000004575 stone Substances 0.000 title description 2
- 238000000137 annealing Methods 0.000 title 1
- 238000000034 method Methods 0.000 claims abstract description 47
- 238000010438 heat treatment Methods 0.000 claims abstract description 35
- 150000002500 ions Chemical class 0.000 claims abstract description 25
- 239000010432 diamond Substances 0.000 claims abstract description 22
- 239000013078 crystal Substances 0.000 claims abstract description 20
- 229910003460 diamond Inorganic materials 0.000 claims abstract description 17
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims abstract description 12
- 239000001301 oxygen Substances 0.000 claims abstract description 12
- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 12
- 238000005498 polishing Methods 0.000 claims abstract description 10
- 229910052594 sapphire Inorganic materials 0.000 claims abstract description 10
- 239000010980 sapphire Substances 0.000 claims abstract description 10
- 229910021645 metal ion Inorganic materials 0.000 claims abstract description 3
- 238000007654 immersion Methods 0.000 claims abstract 4
- 239000011261 inert gas Substances 0.000 claims abstract 2
- 229910052755 nonmetal Inorganic materials 0.000 claims abstract 2
- 239000007789 gas Substances 0.000 claims description 8
- 239000003086 colorant Substances 0.000 claims description 6
- 239000000463 material Substances 0.000 claims description 6
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 4
- 230000035876 healing Effects 0.000 claims description 4
- 239000000843 powder Substances 0.000 claims description 4
- 239000002253 acid Substances 0.000 claims description 3
- 229910052786 argon Inorganic materials 0.000 claims description 3
- 229910052757 nitrogen Inorganic materials 0.000 claims description 3
- 229910052792 caesium Inorganic materials 0.000 claims description 2
- 229910018072 Al 2 O 3 Inorganic materials 0.000 claims 1
- 238000002425 crystallisation Methods 0.000 claims 1
- 230000008025 crystallization Effects 0.000 claims 1
- 238000007599 discharging Methods 0.000 claims 1
- 238000000265 homogenisation Methods 0.000 claims 1
- 230000000630 rising effect Effects 0.000 claims 1
- 230000035939 shock Effects 0.000 claims 1
- 239000010437 gem Substances 0.000 abstract description 13
- 230000000694 effects Effects 0.000 abstract description 9
- 229910001751 gemstone Inorganic materials 0.000 abstract description 8
- -1 sapphires Substances 0.000 abstract description 2
- 239000011259 mixed solution Substances 0.000 abstract 1
- 238000009792 diffusion process Methods 0.000 description 7
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 6
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 4
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 3
- 238000010586 diagram Methods 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
- 229910052751 metal Inorganic materials 0.000 description 3
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 2
- 230000000903 blocking effect Effects 0.000 description 2
- 238000004042 decolorization Methods 0.000 description 2
- 238000007598 dipping method Methods 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 230000005855 radiation Effects 0.000 description 2
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 1
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 239000010953 base metal Substances 0.000 description 1
- 229910052796 boron Inorganic materials 0.000 description 1
- TVFDJXOCXUVLDH-UHFFFAOYSA-N caesium atom Chemical compound [Cs] TVFDJXOCXUVLDH-UHFFFAOYSA-N 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 229910002092 carbon dioxide Inorganic materials 0.000 description 1
- 239000001569 carbon dioxide Substances 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 239000010941 cobalt Substances 0.000 description 1
- 229910017052 cobalt Inorganic materials 0.000 description 1
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 1
- 239000010431 corundum Substances 0.000 description 1
- 229910052593 corundum Inorganic materials 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 238000010884 ion-beam technique Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 229910052744 lithium Inorganic materials 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 1
- 239000010453 quartz Substances 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/0027—Ion-implantation, ion-irradiation or ion-injection
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/0072—Heat treatment
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Ceramic Engineering (AREA)
- Materials Engineering (AREA)
- Structural Engineering (AREA)
- Organic Chemistry (AREA)
- Physics & Mathematics (AREA)
- Thermal Sciences (AREA)
- Health & Medical Sciences (AREA)
- Toxicology (AREA)
- Adornments (AREA)
- Crystals, And After-Treatments Of Crystals (AREA)
Abstract
본 발명은 보석 및 준보석결정(단결정)의 발색방법을 나타낸 것으로 특히 천연 또는 합성 다이아몬드, 사파이어, 수정의 발색방법에 관한 것이다, 목적은 이러한 보석 및 준보석 결정에 대하여 안전하고 일정하게 색 변화와 색 향상을 목적으로 하며 흑색, 갈색 및 청색의 발색효과를 얻을 수 있는 발색방법을 제공하는 것이다. 그 구성은 다이아몬드, 사파이어, 수정 등을 소정형상을 갖는 시편으로 연마하는 연마단계와; 상기 연마단계에서 연마된 시편을 이온주입장치 내 홀더에 시편을 장착시키고 이온주입장치 내 이온원으로부터 소정의 비금속 또는 금속 이온을 발생시켜 인출하여 소정의 전압을 가해 인출한 이온을 가속시켜 홀더에 장착된 시편에 이온을 주입시키는 단계; 이온이주입된 소정형상의 시편을 보우트에 넣어 전기로에 넣고, 진공 또는 소정량의 불활성 가스 또는 산소가 공급되는 상태로 분위기를 조절하면서 소정시간동안 소정온도까지 온도를 상승시킨 후 상승된 목표온도를 소정시간동안 유지시키고 이어서 소정시간동안 실온으로 하강시키는 열처리단계와; 상기 열처리단계에서 열처리가 완료된 시편을 혼합용액에 침지시켜 시편상의 잔류물을 제거하는 침지단계와; 목적하는 표면광택을 위해 재연마 하는 단계로 구성되는 것을 특징으로 한다.The present invention shows a method of coloration of gemstones and semi-precious crystals (single crystals), and more particularly, a method of coloration of natural or synthetic diamonds, sapphires, and crystals. An object of the present invention is to provide a color development method for achieving color development effects of black, brown, and blue. The configuration includes a polishing step of polishing diamond, sapphire, crystal, etc. into a specimen having a predetermined shape; The specimen polished in the polishing step is mounted on the holder in the ion implanter, and extracted by generating a predetermined non-metal or metal ion from the ion source in the ion implanter, applying a predetermined voltage to accelerate the extracted ion to be mounted on the holder. Implanting ions into the prepared specimen; Put a specimen of a predetermined shape into which the ion is implanted, put it in an electric furnace, raise the temperature to a predetermined temperature for a predetermined time while controlling the atmosphere with a vacuum or a predetermined amount of inert gas or oxygen, and then raise the target temperature. A heat treatment step of maintaining for a predetermined time and then lowering to room temperature for a predetermined time; An immersion step of removing the residue on the specimen by immersing the specimen after the heat treatment in the heat treatment step in the mixed solution; It is characterized by consisting of a step of regrinding for the desired surface gloss.
Description
본 발명은 보석 및 준보석의 발색방법에 관한 것으로, 더욱 상세하게는 천연 또는 합성 다이아몬드, 사파이어, 수정 등에 대하여 결정의 손상 없이 매우 안전하고 일정하게 발색시키는 방법으로 흑색, 갈색 및 청색을 포함한 소정의 발색효과를 얻을 수 있는 상기의 보석 및 준보석 발색방법에 관한 것이다.The present invention relates to a method for the coloring of gems and semi-precious stones, and more particularly, to a method of coloring a natural or synthetic diamond, sapphire, crystals, etc. without damaging the crystals in a very safe and constant manner, including black, brown and blue. The present invention relates to a method of coloring a jewel and a semiprecious gem, which can obtain a coloring effect.
보석의 가치에 영향을 미치는 요소 중 색상은 가장 중요한 요소의 하나이고색상의 희귀성, 균일성 및 수요자의 요구에 부합하는 색은 보석의 가치에 지대한 영향을 미친다. 그러나 천연 보석은 그 양이 적고 색상 또한 다양하지 못한 경우가 대부분이어서 색상의 발색 및 조절하는 기술개발은 높은 부가가치 창출을 위해 필수적이다. 다이아몬드는 투명한 무색에서 검은색까지 거의 모든 색으로 산출된다. 이중에서 불순물의 혼입이 없는 무색의 다이아몬드나 희귀한 색을 내는 것일수록 높은 가치가 있으나 그 양이 매우 적고, 공업용으로 사용하기 위해 인공적으로 합성된 다이아몬드는 촉매로 사용된 물질등이 잔류하여 불순물을 포함하고 있고 다양한 색을 발색하지 못하며 진황색등 특정의 색을 띠게된다. 이 경우 강도와 내산성 등 보석 물성에는 변화가 없으나 보석으로써의 경제적가치는 크게 떨어진다. 사파이어와 수정의 경우도 상기 다이아몬드의 경우와 마찬가지로 다양한 색으로 발색시킴으로 해서 높은 부가가치를 창출이 가능하다.Color is one of the most important factors influencing the value of jewelry, and color scarcity, uniformity, and color that meets the needs of the consumer have a great influence on the value of the jewelry. However, since natural gemstones are small in amount and color is not diverse, development of technology to develop and control color is essential for creating high added value. Diamonds are produced in almost any color, from clear colorless to black. Among them, the more colorless diamond or rare color without impurities, the more valuable it is, but the amount is very small, and the artificially synthesized diamond for industrial use remains impurity due to the material used as catalyst. It does not develop a variety of colors and has a specific color such as dark yellow. In this case, there is no change in the properties of the gems such as strength and acid resistance, but the economic value of the gems is greatly reduced. In the case of sapphire and crystal, as in the case of the diamond, it is possible to generate high added value by developing in various colors.
따라서, 당해 기술분야에서는 천연 및 합성다이아몬드, 사파이어 및 수정 등에 인위적으로 색을 부가하거나 제거하여 상기와 같은 문제점을 극복하는 방법을 개발하였다.Therefore, the art has developed a method for overcoming the above problems by artificially adding or removing color to natural and synthetic diamond, sapphire and crystal.
종래의 보석 및 준보석 발색방법으로는 방사능조사법, 표면확산법, 열처리법, 이온주입법 등이 있다.Conventional gem and semiprecious color development methods include radioactivity irradiation, surface diffusion, heat treatment, ion implantation, and the like.
상기와 같은 종래의 발색방법 중 방사능조사법은 α선이나 γ선을 보석 표면부에 노출시켜 점결함을 유발시킴으로서 색을 내는 원리인데, 방사능이 보석에서 계속 방출되므로 반감기를 고려한 안전한 수치까지 내려오기까지 10년 이상의 많은 시간이 소요되어 상용화하기 어려운 단점이 있다. 표면확산법은 단결정 주변에 분말 또는 액상형태의 금속 성분을 위치시키고 특정온도로 온도를 상승시켜 열확산에 의해 표면부로부터 금속 성분을 확산시키는 방법으로서 경제적인 면에서 장점이 있지만 면 방향에 따른 확산정도의 차이로 인한 불균일한 색상분포와 제한적인 분말확산원은 큰 단점으로 작용한다. 열처리법은 가장 오래된 단결정 처리법으로 다양한 색으로의 발색이 어려운 단점이 있다. 이온주입법은 기체 또는 금속이온을 고진공하에서 가속시켜 시편 표면에 주입하는 방법으로 이온의 종류에 따라 다양한 발색이 가능한 특징이 있다. 그러나 고가 이온주입설비가 필요하고 이온주입의 깊이가 표면으로부터 1 ㎛ 이내로 한정되어 최종색상의 질감이 천연석보다 나쁘고 표면 손상이 진행되는 단점이 있다.Radiation irradiation method of the conventional color development method as described above is a principle to give a color by causing α- or γ-rays exposed to the surface of the jewelry to cause defects, since the radiation continues to be emitted from the jewelry until the safe value considering the half-life until 10 It takes a lot of time more than a year has a disadvantage that is difficult to commercialize. The surface diffusion method is a method of dispersing a metal component from a surface part by thermal diffusion by placing a metal component in powder or liquid form around a single crystal and raising the temperature to a specific temperature. Uneven color distribution and limited powder diffusion sources due to differences are a major disadvantage. Heat treatment method is the oldest single crystal treatment method has a disadvantage in that it is difficult to develop a variety of colors. Ion implantation is a method in which gas or metal ions are accelerated under high vacuum to be injected onto the surface of the specimen. However, expensive ion implantation equipment is required, and the depth of ion implantation is limited to within 1 μm from the surface, so that the final color texture is worse than natural stone and surface damage proceeds.
따라서, 본 발명은 상기와 같은 종래의 인공발색방법의 문제점을 고려하여 안출한 것으로써, 그 목적은 다이아몬드, 사파이어, 수정 등의 보석 및 준보석결정(단결정)에 대하여 결정의 손상 없이 매우 안전하고 일정하게 흑색, 갈색 및 청색 등의 소정의 발색효과를 얻을 수 있는 방법을 제공하는 것이다.Therefore, the present invention has been made in view of the problems of the conventional artificial color development method, the purpose of which is very safe without damage to the crystal for gems and semi-precious crystals (single crystal) such as diamond, sapphire, crystal, etc. It is to provide a method which can obtain a predetermined color development effect such as black, brown and blue constantly.
상기 본 발명의 목적은 발색방법에 있어서, 기존의 표면확산법과 이온주입법의 장점만을 이용해서 기존의 보석에 이온주입된 발색원소를 열처리시의 분위기, 온도, 시간 등의 공정조건을 이용하여 발색효과를 조절하는 발명에 관한 것이다.The object of the present invention is the color development method, using only the advantages of the existing surface diffusion method and ion implantation method using the process conditions such as the atmosphere, temperature, time, etc. during the heat treatment of the coloring element ion implanted in the existing jewelry It relates to the invention to control.
도 1은 본 발명에 따른 다이아몬드의 발색, 발색제거 및 발색조절 공정을 예시하는 블록도.1 is a block diagram illustrating a color development, color removal and color control process of the diamond according to the present invention.
도 2는 본 발명에 따른 이온주입장치 개략도.Figure 2 is a schematic view of the ion implantation apparatus according to the present invention.
♣도면의 주요부분에 대한 부호의 설명♣♣ Explanation of symbols for main part of drawing ♣
1: 이온 발생부 2: 이온 가속부1: ion generator 2: ion accelerator
3: 홀더(holder) 4: 이온 빔3: holder 4: ion beam
5: 진공조 6: 시편5: vacuum 6: specimen
이하, 첨부한 도면을 참조하여 본 발명의 바람직한 실시예에 따른 다이아몬드의 발색방법에 대하여 설명하기로 한다.Hereinafter, with reference to the accompanying drawings will be described with respect to the diamond color development method according to a preferred embodiment of the present invention.
도 1은 본 발명에 따른 다이아몬드의 발색, 발색제거 및 발색조절공정을 예시하는 블록도이고, 도 2는 본 발명에 따른 발색공정중 이온주입단계에 따른 이온주입장치를 예시한 개략도를 도시한 도면이다.1 is a block diagram illustrating the color development, color removal and color control process of the diamond according to the present invention, Figure 2 is a schematic diagram illustrating an ion implantation apparatus according to the ion implantation step of the color development process according to the present invention to be.
본 발명에 따른 발색방법은 연마단계와, 이온주입단계, 열처리단계 및 침지단계로 구성된다.The color development method according to the present invention comprises a polishing step, an ion implantation step, a heat treatment step and a dipping step.
상기 연마단계는 보석 및 준보석 결정을 이온주입 및 열처리 공정 전에 소정형상 [예로써 다이아몬드의 경우 통상의 주얼리컷인 라운드 브릴리언트(round brilliant)] 을 갖는 시편으로 연마하는 단계와 열처리 공정 후 표면 광택향상과 표면 손상치유를 위해 연마제 [다이아몬드, 세슘(Cs), 사파이어(Al2O3) 분말등] 를 이용한 재연마단계를 포함한다.The polishing step is to polish the gem and semi-precious crystals into specimens having a predetermined shape (eg, round brilliant, which is a common jewelry cut for diamond) before ion implantation and heat treatment, and to improve surface gloss after heat treatment. Regrind step using abrasive (diamond, cesium (Cs), sapphire (Al 2 O 3 ) powder, etc.) for the surface damage healing.
상기 이온주입단계는 특정한 이온원을 이용해서 이온을 이끌어내고 여기에 다시 전압을 가해 이온을 가속시켜 홀더(holder)에 장착된 시편 표면에 주입시킨다.The ion implantation step derives ions using a specific ion source, applies voltage to it again, accelerates the ions and injects them onto the surface of the specimen mounted in the holder.
이온물질로, 비금속은 붕소(B), 질소(N2), 탄소(C), 및 산소(O2)를 금속은 리튬(Li), 코발트(Co), 니켈(Ni) 및 철(Fe) 등을 사용할 수 있다. 상기 이온주입단계에 질소 이온을 적용 할 때, 이온을 가속시키기 위한 전압의 범위는 20KeV∼180KeV로 하고 이온 농도는 시간당 1×1015~1×1018ions/cm2로 한다.As the ionic material, the base metal is boron (B), nitrogen (N 2 ), carbon (C), and oxygen (O 2 ). The metal is lithium (Li), cobalt (Co), nickel (Ni) and iron (Fe). Etc. can be used. When applying nitrogen ions to the ion implantation step, the voltage range for accelerating ions is 20KeV ~ 180KeV and the ion concentration is 1 × 10 15 ~ 1 × 10 18 ions / cm 2 per hour.
상기 열처리단계는 두 가지 별도의 공정으로 나눌 수 있는데, 그 하나는 상기 이온주입공정에 의한 발색효과를 높이기 위한 발색공정으로 상기와 같이 셋팅된보우트를 전기로에 넣고, 전기로의 내부를 진공으로 하거나 또는 전기로의 내부에 소정량의 질소(N2) 또는 아르곤(Ar2)등의 산소차단가스를 20 내지 30ccm으로 불어넣어 다이아몬드, 사파이어, 수정 등의 시편 표면에 산소가 차단된 분위기를 만든 상태 하에서 목표온도(200 내지 1800℃)까지 3 내지 5시간 동안 서서히 상승 ( + 0.1∼0.5 ° /분) 시키고, 목표한 온도에 도달되면 최고온도를 3 내지 5시간 동안 유지시킨 후 최고온도에서 실온으로 3 내지 5시간 동안에 걸쳐 서서히 하강 ( - 0.1∼0.5 ° /분) 시킨다. 이러한 열처리 공정을 통해 이온주입의 깊이가 표면으로부터 1 ㎛ 이내 인 것을 열 확산효과로 수 ㎛ 까지 침투시켜 색 향상 효과를 얻으며 이온주입에 의한 표면 손상도 치유된다. 이러한 열처리공정을 반복함으로써 수 mm 까지 확산거리의 증가도 가능하다. 또 다른 하나의 열처리 공정은 발색된 색을 제거하거나 조절하는 공정으로 이온주입공정에 의해 발색된 시편이나 상기 열처리 공정에 의해 발색 향상된 시편을 대기상태 또는 소정량의 산소 (밀폐된 분위기 하에서 산소 분률이 20% 내지 100%)로 조절할 수 있는 분위기 하에서 상기와 같은 열처리 공정을 시행함으로 해서 발색된 색을 제거하거나 발색효과를 감소시킨다. 따라서 상기 발명에 따른 산소분위기 하의 열처리 공정을 통해 발색효과를 감하거나 제거하여 발색공정을 재시도 할 수 있다.The heat treatment step may be divided into two separate processes, one of which is a color development process for enhancing the color development effect by the ion implantation process, and the boat set as described above is placed in an electric furnace, and the inside of the electric furnace is vacuumed or Under the condition that oxygen-blocking gas such as nitrogen (N 2 ) or argon (Ar 2 ) is blown into the electric furnace at 20 to 30 ccm, oxygen is blocked on the surface of the specimen such as diamond, sapphire, crystal, etc. Gradually increase (+ 0.1 to 0.5 ° / min) to temperature (200 to 1800 ° C.) for 3 to 5 hours, and maintain the maximum temperature for 3 to 5 hours after reaching the target temperature and then return to room temperature from the highest temperature to 3 to 5 hours. Slowly descend (−0.1 to 0.5 ° / min) over 5 hours. Through this heat treatment process, the depth of ion implantation is within 1 μm from the surface to penetrate to several μm by the heat diffusion effect to obtain a color enhancement effect, and the surface damage by ion implantation is also healed. By repeating this heat treatment process, it is possible to increase the diffusion distance up to several mm. Another heat treatment process is to remove or control the color of the color. The specimen developed by the ion implantation process or the color improved by the heat treatment process is subjected to the atmospheric state or a predetermined amount of oxygen (the oxygen fraction in a sealed atmosphere). 20% to 100%) by performing the heat treatment process as described above in the atmosphere can be adjusted to remove the color or reduce the color development effect. Therefore, the color development effect may be reduced or eliminated through the heat treatment process under an oxygen atmosphere according to the present invention, and the color development process may be retried.
만약 전기로의 내부에 진공이 아닌 산소차단가스를 공급하여 열처리하는 경우에 있어서는 밀폐된 분위기에서 특정압력을 유지하며, 상기 산소차단가스로는 질소(N2), 아르곤(Ar) 또는 이산화탄소(CO2)가스를 사용하는 것이 바람직하지만 상기가스가 아니더라도 시편의 표면에 산소접촉을 적극 차단할 수 있고, 안전한 것이면 어느 가스를 사용하여도 좋다. 상기 보우트는 알루미나 또는 석영으로 제작된 것을 사용한다.If heat treatment is performed by supplying oxygen blocking gas rather than vacuum to the inside of the electric furnace, a specific pressure is maintained in a closed atmosphere, and the oxygen blocking gas is nitrogen (N 2 ), argon (Ar) or carbon dioxide (CO 2 ). Although it is preferable to use a gas, even if it is not the said gas, oxygen contact can be actively interrupted to the surface of a specimen, and as long as it is safe, any gas may be used. The boat is made of alumina or quartz.
상기 침지단계는 상기 열처리단계에서 열처리가 완료된 시편을 처리용액에 침지시켜 시편상의 잔류물을 제거하는데 이때 상기 처리용액으로는 아세톤 및 산을 사용한다. 표면의 재연마 공정은 열처리 및 이온주입시 표면손상이 있을 경우에 기계적, 화학적으로 표면을 미세 연마하여 목적하는 광택을 낼 수 있다.The dipping step is to remove the residue on the specimen by immersing the specimen after the heat treatment in the heat treatment step in the treatment solution, using acetone and acid as the treatment solution. The surface regrinding process may give a desired gloss by finely polishing the surface mechanically and chemically in case of surface damage during heat treatment and ion implantation.
상기와 같은 구성을 갖는 본 발명에 따른 발색방법을 이용함으로 해서 특히 공업용 다이아몬드로서 희소성이 떨어지는 특정의 색만을 내는 황색 다이아몬드를 흑색 및 청색계열의 소정의 색으로 발색시킬 수 있고, 보석으로서 가치가 떨어지는 천연 다이아몬드에 적용하여 역시 상기의 색으로 발색하고 열처리공정으로 농도를 조절하여 목적하는 발색을 대량으로 한번에 발색시킬 수 있다. 이에 부가하여 이온주입에너지를 1MeV 이상으로 증가시켜 이온주입 깊이를 조절하거나 이에 병행하여 단위면적당 이온주입양을 변화시키면 더욱 다양한 색상의 구현이 가능하다.By using the color development method according to the present invention having the above-described configuration, yellow diamonds which give only a specific color of inferiority, in particular as industrial diamonds, can be colored with a predetermined color of black and blue series, and have a low value as a jewel. By applying it to natural diamonds, the color can also be colored and the desired color can be developed at a time by adjusting the concentration by heat treatment. In addition, by increasing the ion implantation energy to 1MeV or more to control the ion implantation depth or in parallel to this change the amount of ion implantation per unit area can realize a variety of colors.
또 다른 실시예로서 다이아몬드와 동일한 공정(전압의 범위는 20KeV∼180KeV, 이온양은 시간당 1×1015~1×1018ions/cm2) 으로 질소이온을 주입시켜서, 사파이어의 경우에는 투명한 커런덤구조의 사파이어를 흑갈색으로 변화시켰고, 투명한 수정의 경우에도 반투명한 흑갈색으로 변화시키는 것이 가능하였다.In another embodiment, nitrogen is implanted in the same process as diamond (voltage range is 20KeV ~ 180KeV, ion amount is 1 × 10 15 ~ 1 × 10 18 ions / cm 2 ), and in the case of sapphire, a transparent corundum structure Sapphire was changed to blackish brown, and even in the case of transparent crystals it was possible to change to translucent blackish brown.
이상으로 설명한 본 발명에 의하면, 천연 또는 합성 다이아몬드, 사파이어, 수정 등에 대하여 결정의 손상 없이 매우 안전하고 일정하게 발색하는 방법으로 기존의 단순한 이온주입에의한 발색외에 열처리공정을 부가하여 발색향상, 발색제거 등 발색을 조절하여 경제적으로 새롭고 다양한 색상의 구현이 가능하며 보석으로써의 심미적 가치를 향상시킬 수 있는 효과를 갖는다.According to the present invention described above, the color development and color development by adding a heat treatment process in addition to the color development by the conventional simple ion implantation in a way to develop a very safe and constant color without damage to the crystal for natural or synthetic diamond, sapphire, crystal, etc. By controlling the color development such as removal, it is possible to economically implement new and various colors, and it has the effect of improving the aesthetic value as a jewel.
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| EP2772565A3 (en) * | 2013-03-02 | 2014-12-10 | Apple Inc. | Sapphire property modification through ion implantation |
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