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KR920701061A - Quartz-based glass doped with rare earth elements and method of manufacturing the same - Google Patents

Quartz-based glass doped with rare earth elements and method of manufacturing the same

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Publication number
KR920701061A
KR920701061A KR1019910701275A KR910701275A KR920701061A KR 920701061 A KR920701061 A KR 920701061A KR 1019910701275 A KR1019910701275 A KR 1019910701275A KR 910701275 A KR910701275 A KR 910701275A KR 920701061 A KR920701061 A KR 920701061A
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South Korea
Prior art keywords
rare earth
glass
doped
quartz
earth element
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KR1019910701275A
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Korean (ko)
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KR0163195B1 (en
Inventor
아끼라 오요베
가즈노리 나까무라
노부유끼 가기
야스마사 사사끼
Original Assignee
원본미기재
후루까와 덴끼 고교 가부시끼가이샤
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Publication of KR920701061A publication Critical patent/KR920701061A/en
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Publication of KR0163195B1 publication Critical patent/KR0163195B1/en

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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
    • C03C13/00—Fibre or filament compositions
    • C03C13/04—Fibre optics, e.g. core and clad fibre compositions
    • C03C13/045—Silica-containing oxide glass compositions
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    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
    • C03B19/00—Other methods of shaping glass
    • C03B19/14—Other methods of shaping glass by gas- or vapour- phase reaction processes
    • C03B19/1415—Reactant delivery systems
    • C03B19/1438—Reactant delivery systems for delivering and depositing additional reactants as liquids or solutions, e.g. solution doping of the article or deposit
    • C—CHEMISTRY; METALLURGY
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    • C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
    • C03B19/00—Other methods of shaping glass
    • C03B19/14—Other methods of shaping glass by gas- or vapour- phase reaction processes
    • C03B19/1453—Thermal after-treatment of the shaped article, e.g. dehydrating, consolidating, sintering
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
    • C03B37/00—Manufacture or treatment of flakes, fibres, or filaments from softened glass, minerals, or slags
    • C03B37/01—Manufacture of glass fibres or filaments
    • C03B37/012—Manufacture of preforms for drawing fibres or filaments
    • C03B37/014—Manufacture of preforms for drawing fibres or filaments made entirely or partially by chemical means, e.g. vapour phase deposition of bulk porous glass either by outside vapour deposition [OVD], or by outside vapour phase oxidation [OVPO] or by vapour axial deposition [VAD]
    • C03B37/01413—Reactant delivery systems
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    • C03B37/00—Manufacture or treatment of flakes, fibres, or filaments from softened glass, minerals, or slags
    • C03B37/01—Manufacture of glass fibres or filaments
    • C03B37/012—Manufacture of preforms for drawing fibres or filaments
    • C03B37/014—Manufacture of preforms for drawing fibres or filaments made entirely or partially by chemical means, e.g. vapour phase deposition of bulk porous glass either by outside vapour deposition [OVD], or by outside vapour phase oxidation [OVPO] or by vapour axial deposition [VAD]
    • C03B37/01446—Thermal after-treatment of preforms, e.g. dehydrating, consolidating, sintering
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    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
    • C03B37/00—Manufacture or treatment of flakes, fibres, or filaments from softened glass, minerals, or slags
    • C03B37/01—Manufacture of glass fibres or filaments
    • C03B37/012—Manufacture of preforms for drawing fibres or filaments
    • C03B37/014—Manufacture of preforms for drawing fibres or filaments made entirely or partially by chemical means, e.g. vapour phase deposition of bulk porous glass either by outside vapour deposition [OVD], or by outside vapour phase oxidation [OVPO] or by vapour axial deposition [VAD]
    • C03B37/016—Manufacture of preforms for drawing fibres or filaments made entirely or partially by chemical means, e.g. vapour phase deposition of bulk porous glass either by outside vapour deposition [OVD], or by outside vapour phase oxidation [OVPO] or by vapour axial deposition [VAD] by a liquid phase reaction process, e.g. through a gel phase
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    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
    • C03B37/00—Manufacture or treatment of flakes, fibres, or filaments from softened glass, minerals, or slags
    • C03B37/01—Manufacture of glass fibres or filaments
    • C03B37/012—Manufacture of preforms for drawing fibres or filaments
    • C03B37/014—Manufacture of preforms for drawing fibres or filaments made entirely or partially by chemical means, e.g. vapour phase deposition of bulk porous glass either by outside vapour deposition [OVD], or by outside vapour phase oxidation [OVPO] or by vapour axial deposition [VAD]
    • C03B37/018—Manufacture of preforms for drawing fibres or filaments made entirely or partially by chemical means, e.g. vapour phase deposition of bulk porous glass either by outside vapour deposition [OVD], or by outside vapour phase oxidation [OVPO] or by vapour axial deposition [VAD] by glass deposition on a glass substrate, e.g. by inside-, modified-, plasma-, or plasma modified- chemical vapour deposition [ICVD, MCVD, PCVD, PMCVD], i.e. by thin layer coating on the inside or outside of a glass tube or on a glass rod
    • C03B37/01807—Reactant delivery systems, e.g. reactant deposition burners
    • C03B37/01838—Reactant delivery systems, e.g. reactant deposition burners for delivering and depositing additional reactants as liquids or solutions, e.g. for solution doping of the deposited glass
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
    • C03B37/00—Manufacture or treatment of flakes, fibres, or filaments from softened glass, minerals, or slags
    • C03B37/01—Manufacture of glass fibres or filaments
    • C03B37/012—Manufacture of preforms for drawing fibres or filaments
    • C03B37/014—Manufacture of preforms for drawing fibres or filaments made entirely or partially by chemical means, e.g. vapour phase deposition of bulk porous glass either by outside vapour deposition [OVD], or by outside vapour phase oxidation [OVPO] or by vapour axial deposition [VAD]
    • C03B37/018—Manufacture of preforms for drawing fibres or filaments made entirely or partially by chemical means, e.g. vapour phase deposition of bulk porous glass either by outside vapour deposition [OVD], or by outside vapour phase oxidation [OVPO] or by vapour axial deposition [VAD] by glass deposition on a glass substrate, e.g. by inside-, modified-, plasma-, or plasma modified- chemical vapour deposition [ICVD, MCVD, PCVD, PMCVD], i.e. by thin layer coating on the inside or outside of a glass tube or on a glass rod
    • C03B37/01853—Thermal after-treatment of preforms, e.g. dehydrating, consolidating, sintering
    • C—CHEMISTRY; METALLURGY
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    • 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
    • C03C23/00—Other surface treatment of glass not in the form of fibres or filaments
    • C03C23/0095—Solution impregnating; Solution doping; Molecular stuffing, e.g. of porous glass
    • C—CHEMISTRY; METALLURGY
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    • 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
    • C03C3/04—Glass compositions containing silica
    • C03C3/06—Glass compositions containing silica with more than 90% silica by weight, e.g. quartz
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    • 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
    • C03C3/04—Glass compositions containing silica
    • C03C3/076—Glass compositions containing silica with 40% to 90% silica, by weight
    • C03C3/095—Glass compositions containing silica with 40% to 90% silica, by weight containing rare earths
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    • C03C4/00—Compositions for glass with special properties
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    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
    • C03B2201/00—Type of glass produced
    • C03B2201/06—Doped silica-based glasses
    • C03B2201/08—Doped silica-based glasses doped with boron or fluorine or other refractive index decreasing dopant
    • C03B2201/12—Doped silica-based glasses doped with boron or fluorine or other refractive index decreasing dopant doped with fluorine
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    • C03B2201/00—Type of glass produced
    • C03B2201/06—Doped silica-based glasses
    • C03B2201/30—Doped silica-based glasses doped with metals, e.g. Ga, Sn, Sb, Pb or Bi
    • C03B2201/31—Doped silica-based glasses doped with metals, e.g. Ga, Sn, Sb, Pb or Bi doped with germanium
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    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
    • C03B2201/00—Type of glass produced
    • C03B2201/06—Doped silica-based glasses
    • C03B2201/30—Doped silica-based glasses doped with metals, e.g. Ga, Sn, Sb, Pb or Bi
    • C03B2201/34—Doped silica-based glasses doped with metals, e.g. Ga, Sn, Sb, Pb or Bi doped with rare earth metals, i.e. with Sc, Y or lanthanides, e.g. for laser-amplifiers
    • C03B2201/36—Doped silica-based glasses doped with metals, e.g. Ga, Sn, Sb, Pb or Bi doped with rare earth metals, i.e. with Sc, Y or lanthanides, e.g. for laser-amplifiers doped with rare earth metals and aluminium, e.g. Er-Al co-doped
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    • C03C2201/00—Glass compositions
    • C03C2201/06—Doped silica-based glasses
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    • C03C2201/12—Doped silica-based glasses containing boron or halide containing fluorine
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    • 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
    • C03C2201/00—Glass compositions
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    • C03C2201/00—Glass compositions
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    • C03C2201/30—Doped silica-based glasses containing metals
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    • C03C2201/3435—Neodymium
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    • C03C2201/00—Glass compositions
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    • C03C2201/06—Doped silica-based glasses
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    • C03C2201/34—Doped silica-based glasses containing metals containing rare earth metals
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    • Y10S501/00—Compositions: ceramic
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Abstract

내용 없음No content

Description

희토류 원소가 도우프된 석영계 유리 및 그 제조방법Quartz-based glass doped with rare earth elements and method of manufacturing the same

본 내용은 요부공개 건이므로 전문내용을 수록하지 않았음Since this is an open matter, no full text was included.

제1도는 실험예 1에 있어서 소결후의 모재의 X선 회절도, 제2도는 실험예 2에 있어서 소결후의 모재의 X선 회절도, 제3도는 본 발명에 있어서, 소결후의 모재의 X선 회절도.1 is an X-ray diffraction diagram of the base material after sintering in Experimental Example 1, FIG. 2 is an X-ray diffraction diagram of the base material after sintering in Experimental Example 2, and FIG. 3 is an X-ray diffraction diagram of the base material after sintering in the present invention. .

Claims (13)

Al와 F와 함께 도우프된 Sio2계의 호스트 유리에 희토류원소가 첨가되어 있는 것을 특징으로 하는 희토류 원소가 도우프된 석영계 유리.A rare earth element-doped quartz-based glass, wherein a rare earth element is added to a host glass of Sio 2 doped with Al and F. 제1항에 있어서, 상기 호스트 유리는 굴절율 증대용 물질 및 유리의 연화온도를 저하시키는 물질도 포함하고 있는 것을 특징으로 하는 희토류원소가 도우프된 석영계 유리.The quartz-based glass doped with rare earth elements according to claim 1, wherein the host glass also includes a material for increasing the refractive index and a material for lowering the softening temperature of the glass. Al와 F가 함께 도우프된 GeO2-SiO2계의 호스트 유리에 희토류 원소가 첨가되어 있는 것을 특징으로 하는 희토류 원소가 도우프된 석영계 유리.A rare earth element-doped quartz-based glass, wherein a rare earth element is added to a GeO 2 -SiO 2 -based host glass doped with Al and F. 제1항 내지 제3항중 어느 한 항에 있어서, 상기 호스트 유리 중의 F함유량은 0.1~약 1.5중량%인 것을 특징으로 하는 희토류 원소가 도우프된 석영계 유리.The quartz-based glass doped with rare earth elements according to any one of claims 1 to 3, wherein the F content in the host glass is 0.1 to about 1.5% by weight. 제3항에 있어서, 상기 호스트 유리중의 GeO2함유량은 약 20중량%미만인 것을 특징으로 하는 희토류 원소가 도우프된 석영계 유리.4. The quartz-based glass doped with rare earth elements according to claim 3, wherein the GeO 2 content in the host glass is less than about 20% by weight. 제1항 내지 제5항중 어느 한항에 있어서, 상기 호스트 유리에 Er, Nd중 어느 하나의 희토류원소가 첨가되어 있는 것을 특징으로 하는 희토류 원소가 도우프된 석영계 유리.The rare earth element-doped quartz glass according to any one of claims 1 to 5, wherein a rare earth element of either Er or Nd is added to the host glass. 제1항 내지 제6항중 어느 한 항에 있어서, 상기 호스트 유리중의 흐토류원소 농도는 중량으로 약 4000ppm이하이고, A1농도가 중량으로 약50000ppm 이하인 것을 특징으로 하는 희토류원소이고 도우프된 석영계 유리.The rare earth element and the doped quartz system according to any one of claims 1 to 6, wherein the concentration of the H earth element in the host glass is about 4000 ppm or less by weight, and the A1 concentration is about 50000 ppm or less by weight. Glass. 제1항 내지 제7항중 어느 한 항에 있어서, 광섬유, 광도파로 중의 어느하나에 사용되는 것을 특징으로 하는 희토류원소가 도우프된 석영계 유리.8. A quartz-based glass doped with rare earth elements according to any one of claims 1 to 7, which is used for any one of an optical fiber and an optical waveguide. 희토류원소 이온과 알루미늄 이온을 포함하는 용액중에 다공질 유리 모재를 침지하고 그 모재중에 희토류원소, 알리미늄을 침지시키는 도우프공정과, 도우프 공정후의 다공질 유리 모재를 건조해서 그 모재의 기공내에 희토류 원소, 알루미늄의 염을 침적시키든가 또는 상기 침적을 행하고 침적한 염을 산화해서 안정시키는 건조공정 및, 건조공정후의 다공질 유리 모재를 소결 또는 무공화하는 소결공정을 구비하는 희토류 원소가 도우프된 석영계 유리의 제조방법에 있어서, 상기 건조 공정이 종결된 후부터 상기 소결공정이 종결될 때까지 동안에, 불소를 함유하는 분위기중에서 상기 다공질 유리 모재를 가열처리하여 그 모재중에 불소를 도우프하는 볼소 도우프 공정이 개재되어 있는 것을 특징으로 하는 희토류 원소가 도우프된 석영계 유리 제조방법.A dope process in which a porous glass base material is immersed in a solution containing rare earth element ions and aluminum ions, and a rare earth element and aluminum is immersed in the base material; A rare earth element-doped quartz system comprising a drying step of depositing a salt of aluminum or oxidizing and stabilizing the deposited salt, and a sintering step of sintering or nonporousing the porous glass base material after the drying step. In the method for producing glass, the Bolso dope step of heating the porous glass base material in a fluorine-containing atmosphere and dope the fluorine in the base material from the end of the drying step until the end of the sintering step. Manufacture of quartz-based glass doped with rare earth elements characterized by interposition Way. 제9항에 있어서, 상기 건조 공정이 종결된 후부터 상기 소결 공정이 종결될때까지 동안에, 볼소 도우프 공정외에 염소계 가스와 산호를 포함하는 분위기 중에서 다공질 유리 모재를 탈수처리하는 탈수공정도 개재되어 있는 것을 특징으로 하는 희토류원소가 도우프된 석영계 유리 제조방법.10. The method of claim 9, wherein from the end of the drying process until the end of the sintering process, a dehydration step of dehydrating the porous glass base material in an atmosphere containing chlorine-based gas and coral is also included in addition to the Bolso dope process. A method for producing a quartz-based glass doped with rare earth elements. 제9항 또는 제10항에 있어서, 불화 알루미늄의 승화온도보다 저온의 불소함유 분위기 중에서 불소 도우프 공정을 실시하는 것을 특징으로 하는 희토류원소가 도우프된 석영계 유리 제조방법.The method of claim 9 or 10, wherein the fluorine doping process is performed in a fluorine-containing atmosphere at a lower temperature than the sublimation temperature of aluminum fluoride. 제9항 또는 제10항에 있어서, 상기 다공질 유리 모재는 기상반응법, 졸겔법, 분말성형법, 주입 이장법중의 어느 하나에 의해 제작되는 것을 특징으로 하는 희토류 원소가 도우프된 석영계 유리 제조방법.11. The method of claim 9 or 10, wherein the porous glass base material is produced by any one of a gas phase reaction method, sol-gel method, powder molding method, injection separation method, doped quartz-based glass doped with rare earth elements Way. 제9항 또는 제10항에 있어서, 건조공정후의 상기 다공질 유리 모재는 멀라이트와 홍연석의 공융점인 1587±10℃ 이하의 온도에서 무공화기공 폐색할 수 있는 조성을 갖고 있는 것을 특징으로 하는 희토류원소가 도우프된 석영계 유리 제조방법.The rare earth element according to claim 9 or 10, wherein the porous glass base material after the drying process has a composition capable of occluding non-porous pores at a temperature of 1587 ± 10 ° C. or less, which is the eutectic point of mullite and red lead. Method of manufacturing doped quartz-based glass. ※ 참고사항 : 최초출원 내용에 의하여 공개하는 것임.※ Note: The disclosure is based on the initial application.
KR1019910701275A 1990-02-05 1991-02-05 Quartz-based glass doped with rare earth elements and method of manufacturing the same KR0163195B1 (en)

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