KR20210083424A - Chalcogenide ingot manufacturing method - Google Patents

Chalcogenide ingot manufacturing method Download PDF

Info

Publication number
KR20210083424A
KR20210083424A KR1020190174916A KR20190174916A KR20210083424A KR 20210083424 A KR20210083424 A KR 20210083424A KR 1020190174916 A KR1020190174916 A KR 1020190174916A KR 20190174916 A KR20190174916 A KR 20190174916A KR 20210083424 A KR20210083424 A KR 20210083424A
Authority
KR
South Korea
Prior art keywords
chalcogenide
ingot
manufacturing
present
synthesizing
Prior art date
Application number
KR1020190174916A
Other languages
Korean (ko)
Other versions
KR102283586B1 (en
Inventor
변태선
조흥규
이영민
임용균
김경한
함성현
Original Assignee
주식회사 에이치엠오
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 주식회사 에이치엠오 filed Critical 주식회사 에이치엠오
Priority to KR1020190174916A priority Critical patent/KR102283586B1/en
Publication of KR20210083424A publication Critical patent/KR20210083424A/en
Application granted granted Critical
Publication of KR102283586B1 publication Critical patent/KR102283586B1/en

Links

Images

Classifications

    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C3/00—Glass compositions
    • C03C3/32—Non-oxide glass compositions, e.g. binary or ternary halides, sulfides or nitrides of germanium, selenium or tellurium
    • C03C3/321—Chalcogenide glasses, e.g. containing S, Se, Te
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
    • C03B11/00—Pressing molten glass or performed glass reheated to equivalent low viscosity without blowing
    • C03B11/06—Construction of plunger or mould
    • C03B11/08—Construction of plunger or mould for making solid articles, e.g. lenses

Landscapes

  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Organic Chemistry (AREA)
  • Manufacturing & Machinery (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Geochemistry & Mineralogy (AREA)
  • Glass Compositions (AREA)

Abstract

A method for manufacturing a chalcogenide ingot is provided. The method includes the steps of: purifying Ge; weighing purified Ge, Sb, and Se; melting and synthesizing a mixture of Ge, Sb, and Se; and annealing a composite. The melting and synthesizing step is performed in a locking furnace through multi-step heating. An ingot manufactured in this way can be cut into a preform and can be manufactured into an infrared optical lens through molding.

Description

칼코게나이드 잉곳 제조 방법{CHALCOGENIDE INGOT MANUFACTURING METHOD}Method for manufacturing chalcogenide ingot {CHALCOGENIDE INGOT MANUFACTURING METHOD}

본 발명은 칼코게나이드 유리 제조 분야에 관한 것으로서, 보다 상세하게는 몰딩 성형을 통해 렌즈로 제조되는 칼코게나이드 잉곳 제조 방법에 관한 것이다.The present invention relates to the field of manufacturing chalcogenide glass, and more particularly, to a method for manufacturing a chalcogenide ingot manufactured as a lens through molding.

최근 CCTV 카메라, 체열진단기 등에 적외선 광학 렌즈의 이용이 증가하고 있다. 적외선 광학렌즈를 위한 기존의 일반적인 소재는 Ge, Si, ZnSe와 같은 결정질이다. 이를 통상 다이어몬드 터닝 머신과 같은 장비를 이용하여 절삭하여 원하는 치수를 가지는 열상 장비용 광학렌즈로 제조한다. 그러나 이러한 결정질 소재를 이용하고 그를 절삭하는 기존의 방식은 생산 효율이 낮고 비용이 많이 드는 문제점이 있다.Recently, the use of infrared optical lenses is increasing in CCTV cameras and body temperature diagnostic devices. Existing common materials for infrared optical lenses are crystalline such as Ge, Si, and ZnSe. This is usually cut using equipment such as a diamond turning machine to manufacture an optical lens for thermal imaging equipment having desired dimensions. However, the conventional method of using such a crystalline material and cutting it has a problem of low production efficiency and high cost.

근래에는 칼코게나이드계 소재를 합성하여 몰딩 성형을 통해 적외선 광학렌즈를 제조하는 방식이 이용되고 있다. 이와 같은 비정질 칼코게나이드계 소재를 합성하여 바람직한 기계적, 광학적 특성을 얻기 위해서는 새로운 합성 방법이 필요하다.Recently, a method of manufacturing an infrared optical lens through molding by synthesizing a chalcogenide-based material is used. In order to obtain desirable mechanical and optical properties by synthesizing such amorphous chalcogenide-based materials, a new synthesis method is required.

본 발명은 상술한 종래의 문제를 감안한 것으로서, 경제적인 칼코게나이드 잉곳 제조 방법을 제공한다.The present invention provides an economical chalcogenide ingot manufacturing method in consideration of the above-mentioned conventional problems.

본 발명은 칼코게나이드 잉곳 제조방법을 제공하며, 이는: Ge을 정제하는 단계; 정제된 Ge, Sb, 및 Se를 칭량하는 단계; Ge, Sb, 및 Se의 혼합물을 용융하여 합성하는 단계; 및 합성물을 어닐링하는 단계;를 포함한다.The present invention provides a method for manufacturing a chalcogenide ingot, comprising: purifying Ge; Weighing purified Ge, Sb, and Se; synthesizing a mixture of Ge, Sb, and Se; and annealing the composite.

상기 용융하여 합성하는 단계는 락킹로(rocking furnace)에서 수행할 수 있다.The melting and synthesizing step may be performed in a rocking furnace.

상기 용융하여 합성하는 단계는,The melting and synthesizing step,

Figure pat00001
Figure pat00001

의 과정으로 진행할 수 있다.can proceed with the process of

상기 어닐링 단계는,The annealing step is

Figure pat00002
Figure pat00002

의 과정으로 진행할 수 있다.can proceed with the process of

본 발명에 따르면, 경제적인 방식으로 칼코게나이드계 잉곳을 제조할 수 있는 방법이 제공된다. 락킹 로에서 다단계의 과정을 통해 양호한 품질의 칼코게나이드 유리가 합성될 수 있고, 이는 바람직하게 적외선 광학 렌즈로 적용될 수 있다.According to the present invention, there is provided a method capable of manufacturing a chalcogenide-based ingot in an economical manner. Good quality chalcogenide glass can be synthesized through a multi-step process in a locking furnace, which can be preferably applied as an infrared optical lens.

도 1은 본 발명의 칼코게나이드 잉곳 제조방법을 나타내는 공정 플로우이다.
도 2는 본 발명의 잉곳 제조방법으로 얻어진 잉곳을 이용하여 적외선 광학 렌즈를 제조하는 과정의 예시를 보여준다.
도 3은 본 발명의 칼코게나이드 유리 제조방법으로 제조된 적외선 광학렌즈용 잉곳에 대한 사진이다.1 is a process flow showing a chalcogenide ingot manufacturing method of the present invention.
2 shows an example of a process for manufacturing an infrared optical lens using the ingot obtained by the ingot manufacturing method of the present invention.
3 is a photograph of an ingot for an infrared optical lens manufactured by the method of manufacturing a chalcogenide glass of the present invention.

이하 첨부한 도면을 참조하여 본 발명의 실시예를 상세하게 설명한다. 본 발명의 실시예를 설명함에 있어서, 관련된 공지기능 혹은 구성에 대한 구체적인 설명이 본 발명의 요지를 불필요하게 흐릴 수 있다고 판단되는 경우 그 상세한 설명을 생략한다.Hereinafter, embodiments of the present invention will be described in detail with reference to the accompanying drawings. In describing the embodiment of the present invention, if it is determined that a detailed description of a related known function or configuration may unnecessarily obscure the gist of the present invention, the detailed description thereof will be omitted.

본 발명의 칼코게나이드 유리 제조방법은 Ge28Sb12Se60을 용융 합성하는 방법이다. 상기 성분들을 유리 용기를 밀봉하고 락킹로(rocking furnace)에 장입한 후, 다단계의 가열 과정을 통해 용융 합성한다. 이어서, 합성물을 어닐링함으로써 몰딩 성형용의 칼코게나이드 잉곳이 얻어진다.The chalcogenide glass manufacturing method of the present invention is a method of fusion synthesis of Ge 28 Sb 12 Se 60 . The above components are melted and synthesized through a multi-step heating process after sealing the glass container and loading it into a rocking furnace. Then, by annealing the compound, a chalcogenide ingot for molding is obtained.

이하에서는 도면을 참조하여 본 발명의 칼코게나이드 잉곳 제조방법을 설명한다.Hereinafter, a method for manufacturing a chalcogenide ingot of the present invention will be described with reference to the drawings.

도 1은 본 발명의 칼코게나이드 잉곳 제조방법을 나타내는 공정 플로우이다. 도 2는 본 발명의 잉곳 제조방법으로 얻어진 잉곳을 이용하여 적외선 광학 렌즈를 제조하는 과정의 예시를 보여준다. 도 3은 본 발명의 칼코게나이드 유리 제조방법으로 제조된 적외선 광학렌즈용 잉곳에 대한 사진이다.1 is a process flow showing a chalcogenide ingot manufacturing method of the present invention. 2 shows an example of a process for manufacturing an infrared optical lens using the ingot obtained by the ingot manufacturing method of the present invention. 3 is a photograph of an ingot for an infrared optical lens manufactured by the method of manufacturing a chalcogenide glass of the present invention.

이어, Ge28Sb12Se60를 유리 용기에 수용하여 밀봉한 후, 유리 용기를 락킹로에 장입하여 용융 합성 단계를 수행한다.Then, after receiving and sealing Ge 28 Sb 12 Se 60 in a glass container, the glass container is charged into a locking furnace to perform a fusion synthesis step.

구체적으로, 도 1에 나타낸 바와 같이, 먼저 Ge 정제(110)한다.Specifically, as shown in FIG. 1 , first Ge purification 110 is performed.

이어, Ge, Sb, 및 Se를 칭량하여, 유리 용기에 투입한다(120). 용기를 밀봉한 후 락킹로(rocking furnace)에 장입한다(130).Next, Ge, Sb, and Se are weighed and put into a glass container ( 120 ). After sealing the container, it is charged into a rocking furnace (130).

용융 합성 단계는 유리 용기를 락킹(rocking)하면서 다단계의 온도로 가열하여 수행한다. 이를테면, 아래 표 1와 같은 다단계 가열과 자연 냉각을 수행할 수 있다.The melt synthesis step is performed by heating the glass container to a multi-step temperature while rocking. For example, multi-stage heating and natural cooling as shown in Table 1 below may be performed.

상기 용융하여 합성하는 단계는,The melting and synthesizing step, 450 -> 800도450 -> 800 degrees 800도800 degrees 800도
(수평)800 degrees
(level) 800도
(수평->수직)800 degrees
(Horizontal->Vertical) 800도
(수직)800 degrees
(Perpendicular) 800 ->
580도800 ->
580 degrees 580도580 degrees 3시간3 hours 12시간12 hours 20분20 minutes 20분20 minutes 1시간1 hours 2시간30분2 hours 30 minutes 20분20 minutes

이어, 아래 표 2와 같은 조건으로 어닐링 단계(140)를 수행한다.Then, the annealing step 140 is performed under the conditions shown in Table 2 below.

320도320 degrees 320 -> 285도320 -> 285 degrees 285도285 degrees 10분10 minutes 10분10 minutes 2시간2 hours

도 3은 본 발명의 비증류식 정제 과정을 포함하는 칼코게나이드 유리 제조방법으로 제조된 적외선 광학렌즈용 잉곳에 대한 사진이다.3 is a photograph of an ingot for an infrared optical lens manufactured by the method for manufacturing chalcogenide glass including the non-distillation purification process of the present invention.

참고적으로, 이상과 같이 제조된 칼코게나이드 잉곳을 준비(310)하여 아래와 같은 과정을 통해 적외선 광학 렌즈를 제조한다.For reference, the chalcogenide ingot prepared as described above is prepared (310) to manufacture an infrared optical lens through the following process.

이어, 본 발명에서 제조된 잉곳을 컷팅하여 렌즈의 프리폼을 제조하는 단계(320)를 수행한다. 예를 들어 여기서 설명되는 렌즈는 5mm의 적외선 광학 렌즈일 수 있다. 목표하는 광학 렌즈의 치수에 알맞도록 잉곳을 컷팅한다.Next, a step 320 of manufacturing a preform of a lens by cutting the ingot manufactured in the present invention is performed. For example, the lens described herein may be an infrared optical lens of 5 mm. The ingot is cut to fit the dimensions of the target optical lens.

이어 제조된 프리폼을 가열하는 단계(330)를 수행한다. 가열 단계(330)는 다단계의 가열 과정을 포함할 수 있다. 예를 들어, 가열 단계(330)는 285 내지 335℃의 제1가열과, 320 내지 350℃의 제2가열을 포함할 수 있다.Then, a step 330 of heating the manufactured preform is performed. The heating step 330 may include a multi-step heating process. For example, the heating step 330 may include a first heating of 285 to 335 °C, and a second heating of 320 to 350 °C.

제1가열과 제2가열의 가열 온도 범위는 프리폼이 완전히 용융되지 않을 정도에서 형상의 성형이 가능한 상태가 되는 온도 범위이다. 가열은 예를 들어 적외선 램프를 이용할 수 있다.The heating temperature range of the first heating and the second heating is a temperature range in which a shape can be formed to the extent that the preform is not completely melted. Heating may use, for example, an infrared lamp.

계속하여 성형하는 단계(340)를 진행한다. 성형 단계(340)는 몰딩 성형 과정으로서, 제1프레싱과 제2프레싱을 포함할 수 있다.Continue to the molding step 340 proceeds. The forming step 340 is a molding forming process, and may include a first pressing and a second pressing.

성형 후에는 냉각하는 단계(350)를 수행한다. 냉각 단계(350)는 서냉과정인 제1 및 제2 냉각과 급냉과정인 제3냉각을 포함한다.After molding, a cooling step 350 is performed. The cooling step 350 includes first and second cooling, which is a slow cooling process, and a third cooling, which is a rapid cooling process.

각 단계는 50 내지 60초 범위에서 수행하는 것일 수 있다. 또한 각 단계는 챔버 내 10ppm 미만의 산소농도에서 수행하는 것일 수 있다.Each step may be performed in the range of 50 to 60 seconds. In addition, each step may be performed at an oxygen concentration of less than 10 ppm in the chamber.

이상에서 설명한 바와 같이, 본 발명은 경제적인 비용으로 고품질의 적외선 광학 렌즈를 제조할 수 있는 잉곳을 제공할 수 있다. 이렇게 칼코게나이드 유리를 합성하여 잉곳으로 제조한 후 그를 이용하여 몰딩 성형으로 렌즈를 제조한다. 따라서, 적외선 렌즈의 보급확대에 크게 기여할 수 있을 것으로 기대된다.As described above, the present invention can provide an ingot capable of manufacturing a high-quality infrared optical lens at an economical cost. After synthesizing the chalcogenide glass in this way to manufacture an ingot, the lens is manufactured by molding using it. Therefore, it is expected to greatly contribute to the spread of infrared lenses.

이상, 본 발명의 상세한 설명에서는 구체적인 실시예에 관해서 설명하였으나, 본 발명의 범위에서 벗어나지 않는 한도 내에서 여러 가지 변형이 가능함은 당해 분야에서 통상의 지식을 가진 자에게 있어서 자명하다 할 것이다.As mentioned above, although specific embodiments have been described in the detailed description of the present invention, it will be apparent to those of ordinary skill in the art that various modifications are possible without departing from the scope of the present invention.

Claims (4)

Ge을 정제하는 단계;
정제된 Ge, Sb, 및 Se를 칭량하는 단계;
Ge, Sb, 및 Se의 혼합물을 용융하여 합성하는 단계; 및
합성물을 어닐링하는 단계;를 포함하는 칼코게나이드 잉곳 제조방법.purifying Ge;
Weighing purified Ge, Sb, and Se;
synthesizing a mixture of Ge, Sb, and Se; and
Method for producing a chalcogenide ingot comprising; annealing the composite. 청구항 1에 있어서,
상기 용융하여 합성하는 단계는 락킹로(rocking furnace)에서 수행하는 것인 칼코게나이드 잉곳 제조방법.
The method according to claim 1,
The melting and synthesizing step is a chalcogenide ingot manufacturing method that is performed in a rocking furnace.
 청구항 1에 있어서,
상기 용융하여 합성하는 단계는,
상기 용융하여 합성하는 단계는,
Figure pat00003

의 과정으로 진행하는 것인 칼코게나이드 잉곳 제조방법.
The method according to claim 1,
The melting and synthesizing step,
The melting and synthesizing step,
Figure pat00003

A chalcogenide ingot manufacturing method that proceeds with the process of
 청구항 1에 있어서,
상기 어닐링 단계는,
Figure pat00004

의 과정으로 진행하는 것인 칼코게나이드 잉곳 제조방법.The method according to claim 1,
The annealing step is
Figure pat00004

A chalcogenide ingot manufacturing method that proceeds with the process of
KR1020190174916A 2019-12-26 2019-12-26 Chalcogenide ingot manufacturing method KR102283586B1 (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
KR1020190174916A KR102283586B1 (en) 2019-12-26 2019-12-26 Chalcogenide ingot manufacturing method

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
KR1020190174916A KR102283586B1 (en) 2019-12-26 2019-12-26 Chalcogenide ingot manufacturing method

Publications (2)

Publication Number Publication Date
KR20210083424A true KR20210083424A (en) 2021-07-07
KR102283586B1 KR102283586B1 (en) 2021-07-30

Family

ID=76861937

Family Applications (1)

Application Number Title Priority Date Filing Date
KR1020190174916A KR102283586B1 (en) 2019-12-26 2019-12-26 Chalcogenide ingot manufacturing method

Country Status (1)

Country Link
KR (1) KR102283586B1 (en)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2023074993A1 (en) * 2021-10-29 2023-05-04 한국광기술원 Zn containing-composition for infrared-transmitting chalcogenide glass, and method for manufacturing optical glass using same

Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2016052159A1 (en) * 2014-09-30 2016-04-07 カーリットホールディングス株式会社 Chalcogenide glass lens production method

Patent Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2016052159A1 (en) * 2014-09-30 2016-04-07 カーリットホールディングス株式会社 Chalcogenide glass lens production method

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2023074993A1 (en) * 2021-10-29 2023-05-04 한국광기술원 Zn containing-composition for infrared-transmitting chalcogenide glass, and method for manufacturing optical glass using same
KR20230061825A (en) * 2021-10-29 2023-05-09 한국광기술원 Infrared Transmitting Chalcogenide Glass Composition Containing Zn and Glass Manufacturing Method Using the Same

Also Published As

Publication number Publication date
KR102283586B1 (en) 2021-07-30

Similar Documents

Publication Publication Date Title
CN1590332A (en) Precision press-molding preform, process for the production thereof, optical element and process for the production of the optical element
CN1298651C (en) Optical glass, press-molding preform and method of manufacturing same, and optical element and method of manufacturing same
CN1944302A (en) Near-infrared-absorbing glass, near-infrared-absorbing element having the same and image-sensing device
US7837969B2 (en) Method of making large-volume CaF2 single crystals for optical elements with an optic axis parallel to the (100)-or (110)-crystal axis and CaF2 single crystal made thereby
KR102283586B1 (en) Chalcogenide ingot manufacturing method
JP3697008B2 (en) Fluoride crystal and method for producing fluoride crystal lens
US7344595B2 (en) Method and apparatus for purification of crystal material and for making crystals therefrom and use of crystals obtained thereby
US20050227849A1 (en) Optical element made of fluoride crystal
JP2005353718A (en) Window glass of semiconductor package, glass window for semiconductor package, and semiconductor package
WO2017208679A1 (en) Method and device for manufacturing near infrared absorbing glass
US11155487B2 (en) Method for manufacturing infrared-transmissible lens, infrared-transmissible lens, and infrared camera
KR101760039B1 (en) Li2O-Al2O3-SiO2 transparent crystallized glass and the manufacturing method of the same
US8713970B2 (en) Method for producing fluorophosphate glass, glass material for press molding and optical element
JPH11268927A (en) Phosphate glass for precision molding, optical element using the same, and production of optical element
US20080242528A1 (en) Optical glass and method of producing the same
JP2006327837A (en) Fluorite single crystal manufacturing apparatus and method for manufacturing fluorite single crystal using the same
CN1440942A (en) Process for producing glass optical element and method for determining glass component of glass blank
KR102269162B1 (en) Chalcogenide glass manufacturing method including distillation purification process
KR102269165B1 (en) Chalcogenide glass manufacturing method including non-distillation purification process
JP4158252B2 (en) Fluorite single crystal, heat treatment method thereof, and method for producing fluorite single crystal material
NL8402575A (en) METHOD FOR THE MANUFACTURE OF BISMUTHGER MANATIC CRYSTALS
JP2016088753A (en) Crystal production apparatus, single crystal, and optical component
EP4227271A1 (en) Black quartz glass and method of manufacturing same
JP2007031208A (en) ZnS SINTERED COMPACT AND ITS MANUFACTURING METHOD
JP2002308694A (en) Fluoride crystal and method for manufacturing fluoride crystal lens

Legal Events

Date Code Title Description
E701 Decision to grant or registration of patent right