KR100699048B1 - Heat treatment method for blue sapphire - Google Patents
Heat treatment method for blue sapphire Download PDFInfo
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- KR100699048B1 KR100699048B1 KR1020040104516A KR20040104516A KR100699048B1 KR 100699048 B1 KR100699048 B1 KR 100699048B1 KR 1020040104516 A KR1020040104516 A KR 1020040104516A KR 20040104516 A KR20040104516 A KR 20040104516A KR 100699048 B1 KR100699048 B1 KR 100699048B1
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- 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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- A—HUMAN NECESSITIES
- A44—HABERDASHERY; JEWELLERY
- A44C—PERSONAL ADORNMENTS, e.g. JEWELLERY; COINS
- A44C17/00—Gems or the like
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Abstract
본 발명은 천연사파이어 또는 합성사파이어의 표면을 탈색시켜 보다 가치가 높은 반투명 사파이어로 색향상을 시키는 표면가공방법에 대한 발명으로서, 구체적으로는 불투명한 천연 또는 합성 블루 사파이어를 알루미나와 마그네시아와 같은 내화재에 장입시킨 후 산소분압이 높은 산소-프로판 화염 아래에서 30분 내지 2시간 정도 가열하면, 표면부 0.5 mm 내지 1mm 정도를 투명하게 탈색시킬 수 있어, 보다 나은 색조의 천연 또는 합성 사파이어를 얻게 하여, 심미적으로나 경제적으로 보다 가치가 높은 사파이어를 얻을 수 있다.The present invention relates to a surface processing method for decolorizing the surface of natural sapphire or synthetic sapphire to improve color with semitransparent sapphire, which is more valuable. Specifically, opaque natural or synthetic blue sapphire is applied to fireproof materials such as alumina and magnesia. After charging, heating under an oxygen-propane flame with a high oxygen partial pressure for about 30 minutes to 2 hours allows the surface to be decolorized about 0.5 mm to 1 mm in a transparent manner, thereby obtaining natural or synthetic sapphire of better color tone and aesthetics. Higher value sapphire can be obtained both economically and economically.
사파이어, 열처리 공정, 탈색, 산소-프로판 화염Sapphire, heat treatment process, discoloration, oxygen-propane flame
Description
도 1은 내화재에 사파이어를 장입시킨 상태의 단면도1 is a cross-sectional view of a state in which sapphire is charged in a fireproof material
도 2는 표면에 두께 1mm정도가 투명하게 탈색된 사파이어의 단면도Figure 2 is a cross-sectional view of the sapphire discolored transparent about 1mm on the surface
본 발명은 천연사파이어 또는 합성사파이어를 열처리하는 방법에 관한 것이다.The present invention relates to a method for heat treatment of natural or synthetic sapphire.
보석으로서 사용되는 천연 또는 합성 블루 사파이어는 커런덤(Al2O3)단결정에 Fe, Ti가 불순물로 함유되어 푸른색을 나타낸다. 사파이어가 자연상태에서 생성시에는 스트레스 때문에 생긴 국부적인 격자왜곡으로 인하여 내부에 블루이시(bluish)라는 검은 내포물을 포함하여 산출되는 경우가 많다.Natural or synthetic blue sapphire used as a jewel has blue color due to Fe and Ti as impurities in corundum (Al 2 O 3 ) single crystal. When sapphire is produced in its natural state, it is often produced by including black inclusions called bluish due to local lattice distortion caused by stress.
따라서 대부분은 천연 사파이어는 1500℃ 정도의 고온에서 어닐링하여 이러한 블루이시(bluish)를 제거하는데 주로 대기 또는 진공상태에서 CO가 다수 배출되는 코우크스를 이용한 환원성 분위기 아래, 사파이어 보석 전체를 균일하게 열처리 가공하여 보석으로 판매된다.Therefore, most of natural sapphire is annealed at a high temperature of about 1500 ℃ to remove such blueish, and the entire sapphire gem is uniformly heat-treated under a reducing atmosphere using coke, which mainly emits a large amount of CO in air or vacuum. Your jewelry is sold.
합성 사파이어의 경우에는 플레임 퓨전법 등으로 용융상태에서 응고되어 가공되는데, 이 때 성분조절이 용이하지 않아 최종 사파이어가 불투명의 파란색을 띠게 되어 목표하는 색채와 채도, 명도(맑고 투명한 색채를 고급품으로 친다)가 아니더라도 색을 반투명하게 조절하지 못한 채 저가로 판매되는 경우가 많았다.In the case of synthetic sapphire, it is solidified and processed in the molten state by flame fusion method, etc. At this time, the final sapphire becomes opaque blue because the composition is not easy to control. ), They were often sold at low prices without color translucency adjustment.
또한 기존의 사파이어 보석가공에 있어서는 관습적으로 천연원석을 열처리만으로 색을 향상시키는 것은 용인되지만, 발색원소인 Fe, Ti나 다른 제3의 원소를 외부에서 확산시키거나, 이온주입 등의 방법으로 첨가하는 것은 부정적으로 받아들여지므로, 색향상 방법으로는 원석의 성분은 변화시키기 않는 열처리방법이 유일하다고 할 수 있어, 보다 효율적인 열처리에 의한 색향상 기술이 요청되고 있었다.In addition, in conventional sapphire jewelry processing, it is customary to improve the color only by heat treatment of natural gemstones, but it is possible to diffuse Fe, Ti or other third elements, which are chromophores, from the outside, or to add them by ion implantation. Since it is negatively accepted, the only heat treatment method that does not change the components of gemstones is the only color enhancement method, and a color enhancement technique by more efficient heat treatment has been called for.
본 발명은 상기한 종래 기술의 문제점을 해결하여, 열처리 온도, 시간, 분위기의 조성의 조절을 통하여 불투명의 진한 푸른색을 가진 블루사파이어를 반투명의 블루사파이어로 만드는 공정을 제시하여, 보다 심미성이 뛰어나고 경제적으로 가치가 높은 사파이어로 가공하는데 그 목적이 있다.The present invention solves the problems of the prior art, by presenting a process of making the sapphire blue sapphire with a semi-transparent blue sapphire by adjusting the composition of the heat treatment temperature, time, atmosphere, and more excellent esthetics Its purpose is to process economically valuable sapphire.
상기 발명의 목적을 위하여 본 발명에서는 도 1과 같이 산소가 전체 가스 중 부피비로 25% 내지 80%를 차지하는 산소분압이 큰 토오치 화염을 사용하여 사파이어를 가열하게 된다.(도1)For the purposes of the present invention, as shown in FIG. 1, sapphire is heated by using a torch flame having a large oxygen partial pressure such that oxygen occupies 25% to 80% by volume of the total gas.
Al2O3 단결정으로 구성된 사파이어는 내부의 Al의 위치에 불순물 Fe, Ti가 위치하여 이들이 발색원소로서 푸른색을 나타내는 역할을 하게 된다. 이를 고체 화학식으로 나타내면 다음과 같다.In the sapphire composed of Al 2 O 3 single crystals, impurities Fe and Ti are positioned at Al positions inside them, and they play a role of displaying blue color as a coloring element. This is represented by the solid chemical formula.
이 때, 이 반응은 1500℃ 이상에서 용이하게 일어나며, Fe'Al+Ti'Al은 푸른색을 V"+V"Al 은 색이 없는 투명색을 띠게 되므로, 결국 1500℃ 이상의 온도에서 산소의 공급이 충분한 경우 푸른색의 단결정이 투명한 색으로 바뀌게 된다.At this time, this reaction occurs easily at 1500 ° C. or higher, and Fe ' Al + Ti' Al has a blue color and V ″ + V ” Al has a colorless transparent color. If sufficient, the blue single crystal turns into a transparent color.
이 때, 평형상수 Ko는Where equilibrium constant K o is
가 되므로 산소의 압력 즉 Po2가 증가되면 V"o의 농도가 커져서 표면부로부터 산소의 확산이 수반되고 이들 산소가 푸른색을 나타내게 하는 [Fe'Al]를 제거하게 된다.Therefore, when the pressure of oxygen, that is, P o2 is increased, the concentration of V ″ o is increased, which causes diffusion of oxygen from the surface portion and removes [Fe ' Al ], which causes these oxygen to appear blue.
따라서 도1에서 보듯 마그네시아, 알루미나와 같은 내화물(1)에 사파이어를 장입시키고, 산소분압을 크게 하여 1200℃∼1600℃의 산소-프로판 화염 등을 사용하여 30분내지 2시간 정도 가열하여 열처리 하면, 도2에서 점선으로 도시된 바와 같이 사파이어의 표면부 약 0.5mm 내지 1mm 정도만 선택적으로 투명하게 탈색이 가능하다. 이때 가열은 천연임을 특징짓는 루틸실크 내포물의 보존을 위하여 예컨대, 3분에서 6분 사이의 간격 정도로 가열시간을 짧게 하여 여러 번 반복하여 시행할 수도 있다.Therefore, as shown in FIG. 1, when sapphire is charged into a refractory material (1) such as magnesia and alumina, the oxygen partial pressure is increased, and heat-treated after heating for 30 minutes to 2 hours using an oxygen-propane flame at 1200 ° C to 1600 ° C. As shown by a dotted line in FIG. 2, only about 0.5 mm to 1 mm of the surface portion of the sapphire can be selectively transparently discolored. In this case, the heating may be repeated several times by shortening the heating time to an interval of, for example, 3 minutes to 6 minutes for the preservation of the rutile silk inclusions, which characterizes naturalness.
물론 이러한 공정은 예시로서 쉽게 응용되어 기존의 진공 또는 비활성 기체를 사용하여 열처리 하는 공정에서 석유나 LPG를 연소시키는 버너가열 또는 기존의 열처리에 대기압에 존재하는 산소보다 많은 분압산소를 넣은 산소부화송풍방법 등에 의하여 산소를 부화시켜 과산소 분위기에서 산소 분압을 높여 열처리함으로써 동일한 목적을 이룰 수 있으며, 산소 불꽂에서 단순 열처리 뿐만 아니라, BeO와 같이 작은 원자가를 갖는 Be이온을 표면부로부터 용이하게 산소 vacancy에 Be 이온이 단시간에 확산되도록 하는 공정으로도 응용이 가능하다.Of course, this process is easily applied as an example, and an oxygen-enriched blowing method in which burner heating combusts petroleum or LPG in a heat-treatment process using a conventional vacuum or inert gas or a partial pressure oxygen more than oxygen existing at atmospheric pressure in a conventional heat treatment. The same purpose can be achieved by incubating oxygen by heat treatment by increasing oxygen partial pressure in peroxygen atmosphere, and not only simple heat treatment in the oxygen flame, but Be ions having small valences such as BeO Application is also possible as a process for allowing ions to diffuse in a short time.
본 발명은 열처리 방법을 통하여 사파이어의 표면부를 투명하게 처리함으로써 진한 불투명의 푸른색을 가진 저가치의 블루 사파이어를 심미적으로도 경제적으로도 뛰어난 가치를 가친 반투명의 블루 사파이어로 바꿀 수 있게 한다.The present invention makes it possible to convert the low-cost blue sapphire with a deep opacity of blue into a semi-transparent blue sapphire with aesthetic and economical value by transparently treating the surface of the sapphire through a heat treatment method.
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| KR100856109B1 (en) * | 2007-04-05 | 2008-09-02 | 한국원자력연구원 | Method for manufacturing the color controlled sappire |
| JP5463352B2 (en) | 2008-06-12 | 2014-04-09 | コリア アトミック エナジー リサーチ インスティチュート | Method for producing color-adjusted sapphire |
| US11288633B2 (en) | 2010-04-02 | 2022-03-29 | Vivint, Inc. | Door to door sales management tool |
| US8812345B2 (en) | 2010-04-02 | 2014-08-19 | Vivint, Inc. | Door to door sales management tool |
| KR101628209B1 (en) * | 2014-05-21 | 2016-06-08 | 주식회사 사파이어테크놀로지 | Method and apparatus for heat-treating low grade natural sapphire for improving quality |
| KR101658963B1 (en) * | 2014-12-01 | 2016-09-23 | 서울시립대학교 산학협력단 | Method of enhancing qualities of sapphires |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS59174599A (en) | 1983-03-24 | 1984-10-03 | Seiko Epson Corp | Method for synthesizing artificial blue sapphire crystal |
| JPS61261299A (en) | 1985-05-15 | 1986-11-19 | Seiko Epson Corp | Production of star sapphire |
| JPS6287492A (en) | 1985-10-11 | 1987-04-21 | Seiko Epson Corp | Synthesis of star sapphire artificial crystal |
| KR100262497B1 (en) | 1998-04-23 | 2000-09-01 | 강춘근 | A device and method for manufacturing the artificial corundum |
| CN1266112A (en) * | 2000-03-03 | 2000-09-13 | 中国科学院上海光学精密机械研究所 | Decarburization and decoloration annealing method for sapphire crystal |
| KR20030020809A (en) * | 2001-09-04 | 2003-03-10 | 전우용 | Appratus and method of sapphire production by high frequency reduction heating process |
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Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS59174599A (en) | 1983-03-24 | 1984-10-03 | Seiko Epson Corp | Method for synthesizing artificial blue sapphire crystal |
| JPS61261299A (en) | 1985-05-15 | 1986-11-19 | Seiko Epson Corp | Production of star sapphire |
| JPS6287492A (en) | 1985-10-11 | 1987-04-21 | Seiko Epson Corp | Synthesis of star sapphire artificial crystal |
| KR100262497B1 (en) | 1998-04-23 | 2000-09-01 | 강춘근 | A device and method for manufacturing the artificial corundum |
| CN1266112A (en) * | 2000-03-03 | 2000-09-13 | 中国科学院上海光学精密机械研究所 | Decarburization and decoloration annealing method for sapphire crystal |
| KR20030020809A (en) * | 2001-09-04 | 2003-03-10 | 전우용 | Appratus and method of sapphire production by high frequency reduction heating process |
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