WO2016052159A1 - Procédé de production de lentilles en verre de chalcogénure - Google Patents

Procédé de production de lentilles en verre de chalcogénure Download PDF

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Publication number
WO2016052159A1
WO2016052159A1 PCT/JP2015/076018 JP2015076018W WO2016052159A1 WO 2016052159 A1 WO2016052159 A1 WO 2016052159A1 JP 2015076018 W JP2015076018 W JP 2015076018W WO 2016052159 A1 WO2016052159 A1 WO 2016052159A1
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WO
WIPO (PCT)
Prior art keywords
chalcogenide glass
glass material
lens
molding die
softened
Prior art date
Application number
PCT/JP2015/076018
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English (en)
Japanese (ja)
Inventor
松坂充
高瀬公男
千葉一美
Original Assignee
カーリットホールディングス株式会社
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Publication date
Application filed by カーリットホールディングス株式会社 filed Critical カーリットホールディングス株式会社
Priority to JP2016551894A priority Critical patent/JPWO2016052159A1/ja
Publication of WO2016052159A1 publication Critical patent/WO2016052159A1/fr

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    • 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
    • C03B19/00—Other methods of shaping glass
    • C03B19/02—Other methods of shaping glass by casting molten glass, e.g. injection moulding
    • 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
    • C03C4/00—Compositions for glass with special properties
    • C03C4/10—Compositions for glass with special properties for infrared transmitting glass

Definitions

  • the present invention relates to a method for manufacturing a chalcogenide glass lens.
  • Chalcogenide glass is known as a material that transmits visible light and can transmit infrared light up to a long wavelength range.
  • chalcogenide glass has been widely used as an in-vehicle sensor module for thermography and accident prevention.
  • chalcogenide glass is formed in a lens shape and used as an infrared transmissive lens.
  • the chalcogenide glass lens needs to be transmitted to the infrared region on the long wavelength side as much as possible.
  • the transmittance in the infrared region can also be influenced by the method of forming the chalcogenide glass lens. For this reason, the formation method of the chalcogenide glass lens which can permeate
  • JP-A-5-330832 and JP-2012-201523 disclose a method in which a cylindrical chalcogenide glass is cut into a thin piece, or a glass piece crushed from chalcogenide glass is placed in a molding die to form a lens. Is disclosed.
  • an object of the present invention is to provide a method for producing a chalcogenide glass lens that can easily mold a chalcogenide glass lens and has excellent transmittance in the infrared region.
  • a method for producing a chalcogenide glass lens comprising a step of injection molding a softened chalcogenide glass material into a lens shape.
  • the chalcogenide glass material is mounted in a syringe having an injection nozzle at the tip, and the chalcogenide glass material is softened by heating the injection nozzle and the vicinity thereof, and the softened chalcogenide glass material is formed into a lens-shaped cavity.
  • the manufacturing method of [1] which has the process of inject
  • the chalcogenide glass material is rod-shaped, and when heating the rod-shaped chalcogenide glass material in the syringe, the end of the rod-shaped chalcogenide glass material opposite to the injection nozzle is not softened, [2] The manufacturing method according to [2], wherein the rod-shaped chalcogenide glass material is injected into the molding die by pushing the opposite end portion toward the injection nozzle. [4] The method of [2] or [3], wherein the temperature of the molding die is controlled by connecting the molding die to a cooling furnace. [5] The production method of [1] to [4], wherein the chalcogenide glass material contains at least one selected from the group consisting of sulfur, selenium, and tellurium.
  • a chalcogenide glass lens can be easily formed.
  • the chalcogenide glass lens obtained by the production method of the present invention is excellent in transmittance in the infrared region.
  • impurities are hardly mixed in the manufacturing process, and it is difficult to contact oxygen in the air, so that the chalcogenide glass is not easily oxidized.
  • the use of a slow cooling furnace hardly causes distortion on the lens surface.
  • the chalcogenide glass refers to a glass in a glass state having three elements of sulfur, selenium, and tellurium of the periodic table 6B called chalcogen as one of main components.
  • the chalcogenide glass may contain germanium, arsenic, antimony, silicon and the like in addition to the above three elements. Typically, 50 wt% or more of chalcogen is contained. Excellent transmittance in the visible to infrared region.
  • chalcogenide glass has a low softening point (200 to 500 ° C.) and can be molded at a low temperature.
  • the substance used for the chalcogenide glass preferably contains as little oxide as possible from the viewpoint of improving the transmittance in the infrared region.
  • the chalcogenide glass lens produced in the present invention is formed by forming a chalcogenide glass so that the chalcogenide glass is an optical path.
  • a chalcogenide glass is called a chalcogenide glass material as a concept of any shape, and a lens formed in a lens shape is called a chalcogenide glass lens.
  • the chalcogenide glass material is preferably amorphous so that it is not oxidized as much as possible and is not crystallized as much as possible.
  • a rod-shaped material (so-called glass ingot) is suitably used as the chalcogenide glass material before processing into a lens shape.
  • FIG. 1 is a partially transparent schematic cross-sectional view of injection molding in the manufacturing method of the present invention.
  • a chalcogenide glass material is formed into a lens shape by injection molding.
  • Injection molding is a method of obtaining a molded product by injecting a softened material into a molding die and cooling and solidifying it.
  • the chalcogenide glass material is heated and softened, and is injected into a molding die at a temperature (softening point) at which it begins to deform.
  • the chalcogenide glass material 1 is mounted in a syringe 2 having an injection nozzle 5 at the tip, and the injection nozzle 5 and its vicinity are heated by a heater 3 or the like.
  • the chalcogenide glass material 1 is softened, and the softened chalcogenide glass material 1 is injected into a molding die 6 having a lens-shaped cavity.
  • the chalcogenide glass material 1 in the syringe 2 is depicted so as to be seen through.
  • the softening point of chalcogenide glass materials varies depending on the composition.
  • the softening point of chalcogenide glass is approximately 200 to 500 ° C., which is extremely low compared to other optical glass materials.
  • the temperature at which the chalcogenide glass material is heated during injection molding is preferably closer to the softening point of the glass. The higher the temperature, the lower the viscosity of the glass, making it easier to handle.
  • gas may be generated from the chalcogenide glass, which is not suitable for precise molding. It is preferable to heat and mold at as low a temperature as possible (temperature near the softening point).
  • the chalcogenide glass material 1 is usually heated in a syringe 2 equipped with an injection nozzle 5.
  • the injection nozzle 5 of the syringe may be closed or open.
  • the shape of the chalcogenide glass material is not particularly limited, and is preferably a rod shape.
  • a chalcogenide glass lens can be continuously molded by attaching the rod-shaped chalcogenide glass material 1 to the syringe 2 and softening the chalcogenide glass material 1 in the vicinity of the injection nozzle 5.
  • a blanker 4 as shown may be used.
  • the heating of the chalcogenide glass material 1 is performed at a temperature close to the softening point of the chalcogenide glass at and around the injection nozzle 5.
  • the softened chalcogenide glass material 1 is injected into the molding die 6.
  • the injection port of the injection nozzle 5 is closed, the softened chalcogenide glass material 1 is enclosed in the syringe 2.
  • the softened chalcogenide glass material 1 can be injected into the molding die 6.
  • the chalcogenide glass material 1 softened by continuously applying pressure to the chalcogenide glass material 1 is continuously injected from the syringe 2 into the molding die 6. be able to.
  • the form of the molding die 6 is not particularly limited, and usually has an upper die and a lower die, and a lens-shaped cavity is formed between the upper die and the lower die.
  • the injection port of the injection nozzle 5 may be directed between the upper mold and the lower mold or toward the lower mold.
  • the softened chalcogenide glass material 1 can be injected while the upper mold and the lower mold are clamped.
  • a chalcogenide glass lens 1 can be formed by injecting a certain amount of the softened chalcogenide glass material 1 into the lower mold with the upper mold removed, and then fitting the upper mold. .
  • the chalcogenide glass material injected into the molding die may be cooled naturally or may be cooled while controlling the temperature of the molding die 6.
  • the molding die 6 is put in a decooling furnace 7, and firstly heated to a temperature at which the molding die 6 is dissolved and then slowly cooled.
  • solidification during the injection can be prevented.
  • the chalcogenide glass lens with less distortion can be obtained by gradually cooling while controlling the temperature of the molding die 6.
  • the chalcogenide glass is not in contact with oxygen in the air as much as possible when the temperature is high.
  • the chalcogenide glass is in contact with oxygen in the air at a high temperature, the chalcogenide glass is likely to be oxidized and become an oxide, so that the transparency in the infrared region tends to decrease.
  • the production method of the present invention in order to more efficiently prevent the oxidation of the chalcogenide glass, it is preferably performed in an environment having a low oxygen partial pressure, such as an inert gas atmosphere or a vacuum atmosphere.
  • a low oxygen partial pressure such as an inert gas atmosphere or a vacuum atmosphere.
  • implementation in a vacuum atmosphere is more preferable from an economical point of view.
  • the chalcogenide glass lens is preferably made of an amorphous material. Crystallization of the chalcogenide glass is not preferable for the refractive index of the chalcogenide glass lens. According to the production method of the present invention, the chalcogenide glass is difficult to crystallize, and a lens made of amorphous chalcogenide glass can be easily obtained.
  • the chalcogenide glass lens preferably exhibits a high transmittance in a wide wavelength region from the visible region to the infrared region.
  • the transmittance of a lens tends to decrease as the wavelength is increased from visible light.
  • the longest wavelength exhibiting a transmittance of 50% or more is preferably 12 ⁇ m or more, and particularly preferably 12.5 ⁇ m.
  • the chalcogenide glass lens obtained by the production method of the present invention may be used as it is, or the lens surface may be polished. By polishing, a more precise chalcogenide glass lens can be formed.
  • An antireflection film may be disposed on the surface of the chalcogenide glass lens. By disposing an antireflection film, reflection of light can be prevented and a higher transmittance can be obtained.
  • chalcogenide glass ingot (rod-shaped) A rod-shaped (round bar-shaped) ingot was manufactured as a chalcogenide glass material.
  • the composition of the chalcogenide glass lens is as follows. The number is atomic%. (1) Composition 1: Ge 22 As 20 Se 58 (2) Composition 2: Ge 8 Sb 31 Se 61 (3) Composition 3: As 40 Se 60
  • Composition 1 is for Example 1, Comparative Examples 1 and 2, Composition 2 is for Example 2, Comparative Examples 3 and 4, and Composition 3 is for Example 3, Comparative Examples 5 and 6. , using. Specific processing of Examples and Comparative Examples will be described later.
  • the manufacturing method of the compositions 1 and 2 is as follows.
  • the raw materials of the above components were weighed so as to have the target composition, placed in a quartz glass ampoule, and vacuum sealed. Thereafter, the sealed quartz ampule was placed in an electric furnace, heated from room temperature to 650 ° C. at 10 ° C./min, and held for 2 hours. Thereafter, the temperature was raised to 1000 ° C. at 10 ° C./min and held for 10 hours. Thereafter, the quartz ampule was taken out and quenched with cold water. After quenching, annealing was performed by placing in a 300 ° C. furnace for 9 hours. Thus, a rod-shaped (round bar) glass ingot (rod-shaped) having a diameter of 40 mm and a length of 300 mm was obtained.
  • the manufacturing method of the composition 3 is as follows.
  • the raw materials of the above components were weighed so as to have the target composition, placed in a quartz glass ampoule, and vacuum sealed. Thereafter, the sealed quartz ampule was placed in an electric furnace, heated from room temperature to 300 ° C. at 10 ° C./min, and held for 2 hours. Thereafter, the temperature was raised to 650 ° C. at 10 ° C./min, and held for 6 hours. Thereafter, the quartz ampule was taken out and quenched with cold water. After quenching, annealing was performed by placing in a furnace at 200 ° C. for 6 hours. Thus, a rod-shaped (round bar) glass ingot (rod-shaped) having a diameter of 40 mm and a length of 300 mm was obtained.
  • Example 1 A chalcogenide glass lens was produced from a chalcogenide glass ingot (composition 1) by injection molding schematically shown in FIG.
  • the heating temperature in the heater 3 was 360 ° C., and the end of the ingot opposite to the injection nozzle 5 was not heated and was kept solid.
  • the chalcogenide glass material softened in the vicinity of the injection nozzle 5 was injected into the molding die 6 by pushing the end opposite to the injection nozzle 5 with the plunger 4. After injection into the mold 6, the temperature was lowered to room temperature over 6 hours using a slow cooling furnace 7. As a result, a meniscus chalcogenide glass lens having a diameter of 40 mm, an opposing curvature radius of 5 mm, and a thickness of 2.5 mm was obtained.
  • Comparative Example 1 A chalcogenide glass ingot (Composition 1) was cut to a thickness of 3.0 mm and polished to obtain a meniscus chalcogenide glass lens having a diameter of 7 mm, an opposing curvature radius of 5 mm, and a thickness of 2.5 mm.
  • Comparative Example 2 A chalcogenide glass ingot (Composition 1) is cut to a thickness of 3.0 mm, and a preform is produced by using a preform molding die as described in JP 2012-201523 A. By pressing the preform, a meniscus chalcogenide glass lens having a diameter of 7 mm, an opposing curvature radius of 5 mm, and a thickness of 2.5 mm was obtained.
  • Example 2 A chalcogenide glass lens was obtained in the same manner as in Example 1 except that the ingot of the chalcogenide glass was the composition 2 and the heating temperature in the heater 3 was 380 ° C.
  • Comparative Example 4 A chalcogenide glass lens was obtained in the same manner as in Comparative Example 2 except that the ingot of the chalcogenide glass used was the composition 2.
  • Example 3 Example 1 except that the ingot of the composition 3 was used as the chalcogenide glass ingot, the heating temperature in the heater 3 was 230 ° C., and the temperature was lowered to room temperature over 4 hours using the slow cooling furnace 7 after injection. In the same manner, a chalcogenide glass lens was obtained.
  • Example 1 12.8 ⁇ m Comparative Example 1: 11.1 ⁇ m Comparative Example 2: 10.9 ⁇ m Example 2: 12.6 ⁇ m Comparative Example 3: 11.0 ⁇ m Comparative Example 4: 10.8 ⁇ m Example 3: 12.4 ⁇ m Comparative Example 5: 10.8 ⁇ m Comparative Example 6: 10.6 ⁇ m

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

Abstract

La présente invention concerne un procédé de production permettant d'obtenir facilement une lentille en verre de chalcogénure ayant une excellente transmission dans la région infrarouge. Ce procédé de production comporte une étape de formage par extrusion d'un matériau en verre de chalcogénure (1) ramolli en une forme de lentille, en ajustant de préférence le matériau en verre de chalcogénure (1) à l'intérieur d'une seringue (2) équipée d'une buse d'extrusion (5) au niveau de l'extrémité avant de celle-ci, en chauffant la buse d'extrusion (5) et le voisinage de celle-ci, ce qui permet de ramollir le matériau en verre de chalcogénure (1), et d'extruder le matériau en verre de chalcogénure (1) ramolli dans une matrice de moulage (6) ayant une cavité en forme de lentille.
PCT/JP2015/076018 2014-09-30 2015-09-14 Procédé de production de lentilles en verre de chalcogénure WO2016052159A1 (fr)

Priority Applications (1)

Application Number Priority Date Filing Date Title
JP2016551894A JPWO2016052159A1 (ja) 2014-09-30 2015-09-14 カルコゲナイドガラスレンズの製造方法

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JP2014-200396 2014-09-30
JP2014200396 2014-09-30

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WO2016052159A1 true WO2016052159A1 (fr) 2016-04-07

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2018017406A1 (fr) * 2016-07-18 2018-01-25 Corning Incorporated Utilisation de verres de chalcogénure exempts d'arsenic servant à une transformation à chaud
KR20210083424A (ko) * 2019-12-26 2021-07-07 주식회사 에이치엠오 칼코게나이드 잉곳 제조 방법

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH06279040A (ja) * 1993-03-29 1994-10-04 Japan Steel Works Ltd:The 低融点ガラスの成形方法及び低融点ガラス成形品
JPH10101347A (ja) * 1996-09-24 1998-04-21 Fuji Photo Optical Co Ltd 光学部品の射出成形装置及び射出成形方法
JPH10101362A (ja) * 1996-09-30 1998-04-21 Fuji Photo Optical Co Ltd ロッド状光学ガラス
US20030007203A1 (en) * 2001-04-12 2003-01-09 Max Amon IR lens from moldable infrared material
JP2006290738A (ja) * 2005-04-13 2006-10-26 Corning Inc 低粘度押出成形および射出成形のためのカルコゲナイドガラス

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH06279040A (ja) * 1993-03-29 1994-10-04 Japan Steel Works Ltd:The 低融点ガラスの成形方法及び低融点ガラス成形品
JPH10101347A (ja) * 1996-09-24 1998-04-21 Fuji Photo Optical Co Ltd 光学部品の射出成形装置及び射出成形方法
JPH10101362A (ja) * 1996-09-30 1998-04-21 Fuji Photo Optical Co Ltd ロッド状光学ガラス
US20030007203A1 (en) * 2001-04-12 2003-01-09 Max Amon IR lens from moldable infrared material
JP2006290738A (ja) * 2005-04-13 2006-10-26 Corning Inc 低粘度押出成形および射出成形のためのカルコゲナイドガラス

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2018017406A1 (fr) * 2016-07-18 2018-01-25 Corning Incorporated Utilisation de verres de chalcogénure exempts d'arsenic servant à une transformation à chaud
US10519061B2 (en) 2016-07-18 2019-12-31 Corning Incorporated Use of arsenic-free chalcogenide glasses for hot-melt processing
KR20210083424A (ko) * 2019-12-26 2021-07-07 주식회사 에이치엠오 칼코게나이드 잉곳 제조 방법
KR102283586B1 (ko) * 2019-12-26 2021-07-30 주식회사 에이치엠오 칼코게나이드 잉곳 제조 방법

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