WO2019058618A1 - Composition de verre, élément optique mettant en œuvre celle-ci, et dispositif optique - Google Patents

Composition de verre, élément optique mettant en œuvre celle-ci, et dispositif optique Download PDF

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Publication number
WO2019058618A1
WO2019058618A1 PCT/JP2018/014933 JP2018014933W WO2019058618A1 WO 2019058618 A1 WO2019058618 A1 WO 2019058618A1 JP 2018014933 W JP2018014933 W JP 2018014933W WO 2019058618 A1 WO2019058618 A1 WO 2019058618A1
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Prior art keywords
glass
rare earth
glass composition
earth oxide
present
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PCT/JP2018/014933
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English (en)
Japanese (ja)
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幸平 吉本
嘉信 江面
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株式会社ニコン
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Priority to JP2019542978A priority Critical patent/JP7031676B2/ja
Publication of WO2019058618A1 publication Critical patent/WO2019058618A1/fr
Priority to JP2022024448A priority patent/JP7338721B2/ja

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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
    • C03C3/12—Silica-free oxide glass compositions
    • 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
    • C03C4/12—Compositions for glass with special properties for luminescent glass; for fluorescent glass
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01S—DEVICES USING THE PROCESS OF LIGHT AMPLIFICATION BY STIMULATED EMISSION OF RADIATION [LASER] TO AMPLIFY OR GENERATE LIGHT; DEVICES USING STIMULATED EMISSION OF ELECTROMAGNETIC RADIATION IN WAVE RANGES OTHER THAN OPTICAL
    • H01S3/00—Lasers, i.e. devices using stimulated emission of electromagnetic radiation in the infrared, visible or ultraviolet wave range
    • H01S3/14—Lasers, i.e. devices using stimulated emission of electromagnetic radiation in the infrared, visible or ultraviolet wave range characterised by the material used as the active medium
    • H01S3/16—Solid materials
    • H01S3/17—Solid materials amorphous, e.g. glass

Definitions

  • the present invention relates to a glass composition, an optical element using the same, and an optical device.
  • the present invention claims priority to Japanese Patent Application No. 2017-180573 filed on Sep. 20, 2017, and for designated countries permitted to be incorporated by reference to documents, the contents described in that application are: Incorporated herein by reference.
  • Patent Document 1 discloses a laser medium made of a single crystal or ceramic doped with Cr 3 + and Nd 3 + as a material capable of laser oscillation.
  • a first aspect of the present invention is a glass composition containing 40 to 80% of Ga 2 O 3 and 0% to 60% of rare earth oxide in terms of mol%, and having a maximum phonon energy of 730 cm ⁇ 1 or less It is a thing.
  • a second aspect of the present invention is an optical element using the glass composition of the first aspect.
  • a third aspect of the present invention is an optical device comprising the optical element of the second aspect.
  • the present embodiment is an example for describing the present invention, and is not intended to limit the present invention to the following contents.
  • the present invention can be appropriately modified and implemented within the scope of the gist of the present invention.
  • each component is based on the molar% expression on the oxide basis. It is assumed that complex salts such as carbonates, hydroxides, nitrates and hydrous salts used as raw materials of glass constituents are all decomposed at the time of melting to change into oxides and / or fluorides. In addition, the gas component produced by decomposition
  • the glass composition according to the present embodiment is a glass composition containing 40 to 80% of Ga 2 O 3 and 0% to 60% of a rare earth oxide and having a maximum phonon energy of 730 cm ⁇ 1 or less.
  • fluorescent glass in which rare earth ions are doped in glass, is used as a laser medium or phosphor, for reasons such as easiness of production, flexibility of composition, homogeneity, formability, etc., communication, medicine, processing, nuclear power It is used in a wide range of fields. With the diversification of such applications, the demand for higher luminance of fluorescent glass and improvement of luminous efficiency has been increasing in recent years. In such a fluorescent glass, in order to increase the fluorescence intensity per unit volume, it is necessary to increase the concentration of the rare earth ion which is the light emission center.
  • the rare earth ion when the rare earth ion is contained at a high concentration, the glass becomes unstable and devitrification occurs, which makes it difficult to obtain a transparent and homogeneous medium. Furthermore, when the rare earth ion concentration is too high, there is a problem that the phenomenon of decreasing the light emission intensity (concentration quenching) occurs.
  • the multiphonon relaxation rate W nr in a certain transition process can be expressed by the following equation.
  • W nr A ⁇ exp ( ⁇ ⁇ ⁇ E / (h ⁇ / 2 ⁇ )) (Expression) (Here, A and ⁇ are constants unique to the base material, ⁇ E is the energy difference between the light emission start level and the level immediately below it, and h ⁇ / 2 ⁇ represents the maximum phonon energy of the base material.)
  • the nonradiative transition probability tends to increase and the luminous efficiency tends to decrease if the energy between the levels is small. Further, as the maximum phonon energy of the base material is larger, the number of phonons required for the transition of the constant energy interval is reduced, so the non-radiative transition probability is increased, and the luminous efficiency tends to be lowered as well. Therefore, in order to realize high fluorescence intensity and efficiency, it is necessary to select a glass that can contain rare earth at a high concentration, is less affected by concentration quenching, and has a small maximum phonon energy as a base material. It was
  • fluoride glass tends to have a low heat resistance temperature and a poor chemical durability, the application is limited to a part of fibers and the like. Therefore, its use as a medium for solid laser, for example, is difficult. Furthermore, since it is necessary to carry out the synthesis of fluoride glass under inert atmosphere conditions, there are problems such as requiring large and complicated equipment such as a glove box. In addition, oxide glass is desirable from the practical point of view because it has high thermal and chemical durability and is easy to produce, but its maximum phonon energy is larger than that of the above-mentioned fluoride glass, and it is generally crystallized when rare earth is introduced. There is also a problem that it is easy to cause concentration quenching.
  • Ga 2 O 3 has the effect of enhancing the stability of the glass without significantly increasing the phonon energy in the glass composition according to the present embodiment. If this content is too low, this effect is not sufficient. On the other hand, when introduced in excess, the content of the rare earth oxide relatively decreases, and the desired emission intensity can not be obtained. From such a viewpoint, the content of Ga 2 O 3 is 40 to 80%, preferably 45 to 70%, and more preferably 50 to 60%.
  • the rare earth oxide can be appropriately selected according to the target emission wavelength. If the content of this component is small, sufficient luminescence intensity can not be obtained. On the other hand, if this component is introduced in excess, the glass is likely to be devitrified, and the effect of concentration quenching tends to be large. From such a point of view, the total content of such rare earth oxides is more than 0% to 60% or less, preferably more than 0% to 40% or less, and more preferably 0.5 to 30%. And more preferably 5% to 20%.
  • the rare earth oxide As a specific example of the rare earth oxide, at least a light emitting rare earth may be contained, and the type thereof is not particularly limited, but Er 2 O 3 , Yb 2 O 3 , Eu 2 O 3 , Gd 2 O 3 , Tb 2 O 3 , CeO 2 , Pr 2 O 3 , Sm 2 O 3 , Dy 2 O 3 , Ho 2 O 3 , Tm 2 O 3 and the like.
  • the rare earth oxides may be used alone or in combination of two or more. By co-adding two or more species and utilizing energy transfer between the rare earths, it is also possible to obtain a higher fluorescence intensity than when added alone. When two or more types of rare earth oxides are used in combination, at least one of them may function as a luminescent center, and a suitable combination can be selected appropriately in consideration of the optical properties desired as a glass composition.
  • Preferred specific examples of using two or more rare earth oxides in combination include Er 2 O 3 , Yb 2 O 3 , Eu 2 O 3 , Gd 2 O 3 , Tb 2 O 3 , CeO 2 , Pr 2 O 3 , Sm It is selected from one or more selected from the group consisting of 2 O 3 , Dy 2 O 3 , Ho 2 O 3 and Tm 2 O 3 and the group consisting of La 2 O 3 , Y 2 O 3 and Lu 2 O 3 And a glass composition in which one or more of the following are used in combination.
  • Er 2 O 3 , Yb 2 O 3 , Eu 2 O 3 , Gd 2 O 3 , Tb 2 O 3 , CeO 2 , Pr 2 O 3 , Sm 2 O 3 , Dy 2 O 3 , Ho 2 O 3 and Tm 2 O 3 are rare earth oxides (first rare earth oxides) that mainly function as light emitting centers, and La 2 O 3 , Y 2 O 3 and Lu 2 O 3 are themselves However, it is a rare earth oxide (second rare earth oxide) having the effect of suppressing aggregation of other rare earth ions that become the luminescent center and not suppressing concentration quenching although it does not become the luminescent center.
  • the total content of the first rare earth oxide is preferably 0.5 to 40%, more preferably 5 to 35%, and further preferably 10 to 30%. preferable.
  • the total content of the second rare earth oxide is preferably 5 to 50%, more preferably 10 to 40%, and still more preferably 15 to 30%.
  • La 2 O 3 is more preferable as the second rare earth oxide.
  • Er 2 O 3 , Yb 2 O 3 , and Eu 2 O 3 can be used as the rare earth oxide that is the emission center as a preferable combination with the rare earth oxide that is the emission center. And one combination selected from the group consisting of Tb 2 O 3 and La 2 O 3 .
  • the glass composition according to the present embodiment may further contain other optional components.
  • Such an optional component may introduce not only one type but also two or more types.
  • the glass composition according to the present embodiment has a small maximum phonon energy. Its maximum phonon energy is at 730 cm -1 or less, preferably 700 cm -1 or less, more preferably 670cm -1 or less.
  • the glass composition which concerns on this embodiment can be made into the glass which has high thermal resistance as the suitable aspect.
  • the glass transition temperature (T g ) of the glass composition according to the present embodiment is preferably 700 ° C. or more, more preferably 720 ° C. or more, and still more preferably 740 ° C. or more.
  • the glass composition according to the present embodiment can be suitably used as various optical elements.
  • the optical element using the above-mentioned glass composition can be used for a light emitting element, a wavelength conversion element, an optical amplifier, etc.
  • the optical element according to the present embodiment can be suitably used as an optical device provided with the same.
  • the laser medium of a solid-state laser apparatus (refer FIG. 1), the scintillator (refer FIG. 2) which detects a radiation and an ultraviolet-ray, etc. are mentioned, for example.
  • FIG. 1 is a schematic view showing an example of the configuration of a solid-state laser device using the glass composition according to the present embodiment.
  • the solid-state laser apparatus 1 comprises an excitation light source 10, resonators 12 and 14, and a laser medium 16.
  • the laser medium 16 using the glass composition according to the present embodiment is disposed between the resonators 12 and 14 disposed parallel to each other.
  • the resonator 12 transmits excitation light and is designed to totally reflect the laser light L.
  • the resonator 14 is designed to transmit a part of the laser light L.
  • the laser medium 16 one obtained by mirror-polishing a surface of the glass composition according to the present embodiment located in parallel with the resonators 12 and 14 is used.
  • the laser medium 16 is excited by the excitation light source 10, and the laser light L generated thereby is amplified by reciprocating between the resonators 12 and 14 and the laser medium 16. Then, part of the laser light L emitted from the laser medium 16 is extracted to the outside through the resonator 14.
  • the excitation light source 10 for example, a solid laser or a semiconductor laser can be used.
  • FIG. 2 is a schematic view of a scintillation apparatus using the glass composition according to the present embodiment.
  • Scintillation device 2 includes a scintillator 20 with a glass composition according to the present embodiment, and a detector 22 for about detection light L d.
  • the scintillator 20 has its two surfaces arranged parallel to each other polished. Scintillation characteristics can be imparted by converting radiation or ultraviolet light to a detectable wavelength such as visible light. Since the glass composition according to the present embodiment contains a rare earth at a high concentration, sufficient light emission characteristics can be realized even if the glass thickness is reduced. From such a point of view, the glass composition according to the present embodiment and the optical element or optical device using the same are also effective in reducing the size and weight of the device.
  • optical element and the optical device using the glass composition according to the present embodiment are not limited to the solid laser device and the scintillation device described above, and can be used for various devices.
  • any suitable method can be adopted.
  • a manufacturing method using a floating furnace can be mentioned.
  • the usable floating furnace is not particularly limited, and examples thereof include an electrostatic type, an electromagnetic type, a sonic type, a magnetic type, a gas jet type and the like.
  • a gas jet type floating furnace is preferable for oxide melting.
  • the glass-making feedstock to be used is not specifically limited, For example, an oxide, a hydroxide, carbonate, nitrate, a sulfate, a phosphate etc. can be used.
  • a manufacturing method using a gas jet floating furnace will be described as an example of the manufacturing method.
  • FIG. 3 shows a schematic view of a gas jet floating furnace.
  • FIG. 3A is a schematic view of the entire configuration of the floating furnace
  • FIG. 3B is an enlarged schematic view of a pedestal on the stage of the gas jet floating furnace.
  • the raw material M is disposed on a pedestal 302 on the stage 301.
  • the laser light L emitted from the laser light source 303 is irradiated to the raw material M via the mirror 304 and the mirror 305.
  • the temperature of the raw material M heated by the irradiation of the laser light L is monitored by the radiation thermometer 306.
  • the output of the laser light source 303 is controlled by the computer 307 based on the temperature information of the raw material M monitored by the radiation thermometer 306.
  • the state of the raw material M is imaged by the CCD camera 308, which is output to the monitor 309 (see FIG. 3A).
  • a laser light source a carbon dioxide gas laser can be used, for example.
  • the raw material M floats by the gas fed to the pedestal 302 (see FIG. 3B).
  • the flow rate of the gas fed into the pedestal 302 is controlled by the gas flow rate regulator 310.
  • non-contact heating with laser light L can be performed in a state where the raw material M is suspended by injecting a gas from a nozzle (not shown) provided with a conical hole.
  • a gas from a nozzle not shown
  • the raw material M melts, it becomes spherical or ellipsoidal by its own surface tension, and floats in that state. Thereafter, when the laser light L is shut off, the raw material in the melt state is cooled and a transparent glass is obtained.
  • the kind of gas is not specifically limited, A well-known thing can be employ
  • the shape of the nozzle and the heating method are not particularly limited, and known methods can be appropriately adopted.
  • the composition system as in this embodiment has been difficult to vitrify so far.
  • a large amount of a network forming oxide such as SiO 2 , B 2 O 3 , P 2 O 5 , GeO 2 or the like is included to form a glass. Need to raise.
  • all of these network-forming oxides have high phonon energy, they can be a factor that increases multiphonon relaxation loss.
  • crystallization inhomogeneous nucleation
  • it can not be vitrified.
  • the present embodiment even if the content of the network-forming oxides such as SiO 2 , B 2 O 3 , P 2 O 5 , GeO 2 and the like is reduced, or the network-forming oxides such as these can be used. A glass having excellent physical properties can be realized without being substantially contained.
  • the glass composition according to the present embodiment has a small maximum phonon energy and can contain a high concentration of rare earth atoms. Furthermore, it is also possible to reduce the OH concentration in the glass by using a dry gas for floating. Thereby, it is possible to reduce the loss due to the cross relaxation of the OH group and the radiative transition, particularly for the purpose of obtaining fluorescence in the mid-infrared region. As a result, it is possible to obtain a glass material having excellent light emission intensity and light emission efficiency. When the fluorescent glass is used, the Stokes shift is wide, and excitation light can be emitted to a wide wavelength range.
  • the glass composition was produced according to the following procedures. First, raw materials selected from oxides, hydroxides, carbonates, nitrates, sulfates, phosphates and the like were weighed so as to have a predetermined chemical composition, and then mixed in an alumina mortar. The mixture was uniaxially pressed at 20 MPa to form cylindrical pellets. And the obtained pellet was baked at 1200 degreeC and air
  • the sintered body was roughly crushed and placed on a pedestal 302 of a gas jet floating furnace 3 shown in FIGS. 3A and 3B. Then, the raw material was melted by irradiating the carbon dioxide gas laser from above while injecting dry oxygen gas. The melted raw material becomes approximately spherical by its own surface tension, and floats at the pressure of the gas. Furthermore, when the raw material was completely melted, it was cooled by shutting off the laser output to obtain glass.
  • the optical glass which concerns on a comparative example was produced in the following procedures. First, glass raw materials such as oxides, hydroxides, phosphoric acid compounds (phosphate, orthophosphoric acid, etc.), carbonates, and nitrates are prepared so as to have the chemical compositions (mol%) described in Tables 5-8. Weighed. Next, the weighed raw materials were mixed, charged into a platinum crucible, melted at a temperature of 900 to 1200 ° C. for about 1 hour, and stirred and homogenized. Thereafter, the temperature was lowered to an appropriate temperature, and then cast into a mold or the like, and gradually cooled to obtain each sample.
  • glass raw materials such as oxides, hydroxides, phosphoric acid compounds (phosphate, orthophosphoric acid, etc.), carbonates, and nitrates are prepared so as to have the chemical compositions (mol%) described in Tables 5-8. Weighed. Next, the weighed raw materials were mixed, charged into a platinum crucible, melted at a temperature
  • the glass transition temperature (T g ) of the glass was measured using a differential thermal analyzer (Rigaku, Thermoplus EVO 2 TG 8121) at a temperature rising rate of 10 ° C./minute in an air atmosphere.
  • the maximum phonon energy of the glass was measured by a reflection method using a micro infrared spectrometer (manufactured by Thermo, Nicoleti N10).
  • Example 1 shows component compositions (expressed as molar percentage based on oxide), presence or absence of devitrification, glass transition temperature (T g ), maximum phonon energy (h ⁇ ) for Examples 1 to 5 containing Er 2 O 3 as a luminescent center. / 2 ⁇ ) and the amount of OH ( ⁇ OH ) are shown.
  • FIG. 4 shows the fluorescence spectrum of the 4 I 11/2 ⁇ 4 I 13/2 transition (excitation 980 nm, fluorescence 2.7 ⁇ m) of Examples 1 to 5.
  • fluorescence glass of each embodiment can contain Er 2 O 3 without devitrification at least 20% and high T g, that the maximum phonon energy is small, confirmed respectively.
  • the OH concentration was as small as 0.15 cm -1 or less.
  • the fluorescence intensity of 2.7 ⁇ m increases with the Er 2 O 3 concentration and is maximum at 10%.
  • Table 2 shows the component compositions (expressed in terms of mol% based on oxide), presence or absence of devitrification, glass transition temperature (T g ), and maximum phonon energy (Examples 6 to 11) containing Yb 2 O 3 as a luminescent center. h ⁇ / 2 ⁇ ) is shown.
  • FIG. 5 shows fluorescence spectra excited at 980 nm for Examples 6-11.
  • the fluorescent glass of each example can contain Yb 2 O 3 at high concentration without devitrification, that T g is high, and the maximum phonon energy is small.
  • the fluorescence intensity at 1040 nm showed the maximum value when the Yb 2 O 3 content was 5%.
  • Table 3 shows the component compositions (expressed as molar percent based on oxide), presence or absence of devitrification, glass transition temperature (T g ), maximum phonon energy (h ⁇ ) for Examples 12 to 17 containing Eu 2 O 3 as a luminescent center. / 2 ⁇ ) and a fluorescent color are shown.
  • FIG. 6 shows fluorescence spectra excited with 365 nm light for Examples 12-17.
  • each example can be contained at a high concentration Eu 2 O 3 without devitrification, that high T g, that the maximum phonon energy is small, was confirmed respectively.
  • strong red light emission was obtained in all by 365 nm excitation. From FIG. 6, it was confirmed that the fluorescence intensity at 620 nm increased with the Eu 2 O 3 content and was maximum at 25%.
  • Example 18 to 22 Table 4 shows component compositions (displayed as mol% based on oxide), presence or absence of devitrification, glass transition temperature (T g ), and maximum phonon energy (h ⁇ ) for Examples 18 to 22 containing Tb 2 O 3 as a luminescent center. / 2 ⁇ ) and a fluorescent color are shown.
  • T g glass transition temperature
  • h ⁇ maximum phonon energy
  • the glass composition of each example can contain Tb 2 O 3 at a high concentration without devitrification, has a high T g and has excellent heat resistance, and has a small maximum phonon energy, so it is non-radiative relaxation. It was confirmed that the losses could be kept low respectively. Furthermore, it was confirmed that, with the glass subjected to the reduction annealing treatment, light emission can be obtained with a color tone depending on the blue-green to orange and Tb 2 O 3 content when excited at 375 nm.
  • FIG. 8 shows the fluorescence spectra of Comparative Examples 4 and 5 (spectrum conditions: excitation at 365 nm and 375 nm, respectively) and the fluorescence spectra of Examples 16 and 20. It was confirmed from FIG. 8 that the glass of the present example exhibits high-intensity fluorescence with respect to the glass of the comparative example.

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  • Engineering & Computer Science (AREA)
  • Geochemistry & Mineralogy (AREA)
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Abstract

L'invention concerne une composition de verre qui comprend 40 à 80% d'un Ｇａ２Ｏ３ et plus de 0% à 60% d'un oxyde de terres rares, et qui présente une énergie de phonon maximale inférieure ou égale à ７３０ｃｍ－１.
PCT/JP2018/014933 2017-09-20 2018-04-09 Composition de verre, élément optique mettant en œuvre celle-ci, et dispositif optique WO2019058618A1 (fr)

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JP2022024448A JP7338721B2 (ja) 2017-09-20 2022-02-21 ガラス組成物、それを用いた光学素子及び光学装置

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111510100A (zh) * 2020-05-08 2020-08-07 中山大学 一种基于氧化镓薄膜的压电谐振器及其制备方法

Citations (4)

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Publication number Priority date Publication date Assignee Title
JPH03295828A (ja) * 1990-04-12 1991-12-26 Hoya Corp アップコンバージョンガラス
US5232879A (en) * 1992-08-06 1993-08-03 Corning Incorporated Alkali metal lanthanum gallate glasses
WO2007069730A1 (fr) * 2005-12-16 2007-06-21 Central Glass Company, Limited Materiau et dispositif d'emission de lumiere visible
JP2009286681A (ja) * 2008-05-30 2009-12-10 Ohara Inc 発光性ガラスおよび発光性結晶化ガラス

Family Cites Families (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP4421001B2 (ja) * 1998-04-01 2010-02-24 株式会社住田光学ガラス 長残光および輝尽発光を呈する酸化物ガラス
JP3834670B2 (ja) * 1998-05-13 2006-10-18 株式会社住田光学ガラス 長残光および輝尽発光を呈する酸化物ガラス

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH03295828A (ja) * 1990-04-12 1991-12-26 Hoya Corp アップコンバージョンガラス
US5232879A (en) * 1992-08-06 1993-08-03 Corning Incorporated Alkali metal lanthanum gallate glasses
WO2007069730A1 (fr) * 2005-12-16 2007-06-21 Central Glass Company, Limited Materiau et dispositif d'emission de lumiere visible
JP2009286681A (ja) * 2008-05-30 2009-12-10 Ohara Inc 発光性ガラスおよび発光性結晶化ガラス

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111510100A (zh) * 2020-05-08 2020-08-07 中山大学 一种基于氧化镓薄膜的压电谐振器及其制备方法
CN111510100B (zh) * 2020-05-08 2021-07-02 上海您惦半导体科技有限公司 一种基于氧化镓薄膜的压电谐振器及其制备方法

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