WO2021157135A1 - Ｙａｇセラミックス接合体及びその製造方法 - Google Patents

Ｙａｇセラミックス接合体及びその製造方法 Download PDF

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WO2021157135A1
WO2021157135A1 PCT/JP2020/038554 JP2020038554W WO2021157135A1 WO 2021157135 A1 WO2021157135 A1 WO 2021157135A1 JP 2020038554 W JP2020038554 W JP 2020038554W WO 2021157135 A1 WO2021157135 A1 WO 2021157135A1
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Prior art keywords
yag
ceramics
glass
bonded body
yag ceramics
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English (en)
French (fr)
Japanese (ja)
Inventor
芳樹 山崎
和之 味谷
雅宏 田子
充 三上
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JX Nippon Mining and Metals Corp
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JX Nippon Mining and Metals Corp
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Priority to EP20917282.4A priority Critical patent/EP4023621A4/en
Priority to US17/763,451 priority patent/US12160081B2/en
Priority to JP2021575609A priority patent/JP7503579B2/ja
Priority to CN202080069254.2A priority patent/CN114502520B/zh
Publication of WO2021157135A1 publication Critical patent/WO2021157135A1/ja
Anticipated expiration legal-status Critical
Priority to JP2022206720A priority patent/JP2023029447A/ja
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    • H—ELECTRICITY
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    • H01S3/00—Lasers, i.e. devices using stimulated emission of electromagnetic radiation in the infrared, visible or ultraviolet wave range
    • H01S3/05—Construction or shape of optical resonators; Accommodation of active medium therein; Shape of active medium
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    • H01S3/16—Solid materials
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    • 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
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    • C04B2235/3217—Aluminum oxide or oxide forming salts thereof, e.g. bauxite, alpha-alumina
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Definitions

  • the present invention relates to a YAG (yttrium aluminum garnet) ceramics joint, and more particularly to a YAG ceramics joint in which glass is interposed as a joint layer and a method for producing the same.
  • YAG yttrium aluminum garnet
  • a standard laser is an application that excites a laser medium, which is a phosphor, and amplifies it in an optical cavity sandwiched between optically opposed high reflectance mirrors.
  • YAG ceramics are used as a representative laser medium for high-power lasers.
  • the laser medium is also applied as an amplifier that amplifies the laser light output generated from another medium, except when the laser medium itself serves as an oscillation source.
  • Non-Patent Documents 1 and 2 The development of a light absorbing layer YAG polycrystalline in which Sm is doped around an Nd: YAG polycrystalline material for an amplifier has been reported (Non-Patent Documents 1 and 2). Further, high-power operation has been confirmed by joining a Cr-doped YAG polycrystal to a Yb: YAG laser polycrystal having excellent energy storage (Non-Patent Document 3).
  • YAG semi-lux is exclusively used for high-power lasers, and is a technology for joining YAG ceramics of different dopants and optical glass for light absorption as a light absorption layer to prevent parasitic oscillation to YAG semi-lux in the laser oscillation part. Is required. There is also a demand for large-diameter transparent YAG ceramics, and in order to meet these demands, joining techniques for joining YAG ceramics and joining YAG ceramics and optical glass for light absorption are required.
  • the present invention has been made in view of the above circumstances, and an object of the present invention is a bonded body in which YAG semilux and YAG ceramics are bonded, or a bonded body in which YAG ceramics and optical glass are bonded. Therefore, it is an object of the present invention to provide a bonded body in which the reflection of light at the bonded interface is suppressed and a method for producing the same.
  • An embodiment of the present invention that can solve the above problems is a YAG ceramics bonded body obtained by bonding YAG ceramics with YAG ceramics or optical glass, and includes glass as a bonding layer, and the rate of change in transmittance is 7. It has a gist where it is within%.
  • a bonded body of YAG ceramics and YAG ceramics in which light reflection at the bonding interface is suppressed, or a bonded body of YAG ceramics and optical glass, which has an excellent effect. ..
  • a room temperature joining method has been reported as another method for joining ceramics to each other.
  • the object to be bonded is introduced into a vacuum chamber, and the surface of the contacted surface is irradiated with an atomic beam such as an Ar beam or an ion beam.
  • the irradiated surface is in a state where the surface bonding hands of the elements are exposed, and by bringing the surfaces to be bonded into contact with each other, it is possible to create a strong bond even at room temperature without element diffusion.
  • the adhesive generally has a large coefficient of thermal expansion, and has a problem that the strain becomes large when the temperature is changed.
  • the main component of the adhesive is an organic material, there is a problem that the heat resistance (cold resistance) is inferior.
  • the heat resistance (cold resistance) and light resistance of the skeleton component of the organic substance are deteriorated.
  • nanoparticles are also put into the adhesive, but there is a concern that the bonding strength may be lowered depending on the amount of nanoparticles put.
  • Glass has a solid property that is elastic at room temperature and a liquid property that has a fluid property when the temperature is raised, and is a material with abundant excipients, so that a wide range of material formation is possible.
  • the present invention is characterized in that such glass is used as a bonding layer to produce a bonded body of YAG ceramics or a bonded body of YAG ceramics and another optical material (optical glass).
  • the YAG ceramics bonded body using glass as the bonding layer is extremely useful for laser applications because the reflection of light is suppressed and the transmittance is high at the bonding interface.
  • the ceramics joint according to the present embodiment is a YAG ceramics joint in which YAG ceramics are bonded to YAG ceramics or optical glass, and glass is provided as a bonding layer, and the rate of change in transmittance is within 7%. It is characterized by. More preferably, the rate of change is within 5%, and even more preferably, the rate of change is within 3%.
  • the change rate of the transmittance is defined as the transmittance of light (laser diode) having a wavelength of 650 nm incident on each of the YAG ceramic base material (before bonding) and the YAG ceramic bonding body (after bonding). Is measured and calculated from the following formula.
  • Rate of change in transmittance (transmittance of bonded body) / (transmittance of base material) x 100
  • rate of change of the transmittance is within 7%, it can be said that the reflection of light is sufficiently suppressed at the bonding interface, and it can be used as a laser application.
  • a glass material having a refractive index of 1.71 to 1.91 with respect to light having a wavelength of 650 nm as the glass as the bonding layer.
  • the refractive index of YAG ceramics which is the object to be bonded, depends on the type of dopant, but is about 1.83, and the optical glass used to suppress parasitic oscillation is the same as YAG ceramics, which is a laser medium. Since it has a degree of refractive index, by using a glass material having a refractive index equivalent to these (1.71 to 1.91: wavelength 650 nm) as the bonding layer, light at the bonding interface in the YAG ceramics bonded body is used. The reflection of the glass is suppressed, and an excellent effect of having a high transmittance can be obtained.
  • Glass as a bonding layer is a transparent material containing silicate as the main component, and is an alkali silicate-based glass material, aluminosilicate-based glass, borosilicate-based glass, germanosilicate-based glass, lead-containing glass, and bismuth volate. System glass or the like can be used. Further, considering the bonding process, it is preferable to use glass having a low melting point (melting point: 1500 ° C. or less), but there is no particular problem as long as the refractive index is close to that of YAG ceramics or optical glass even if the melting point is high. .. Further, a crystallized part or all of the glass material can be used.
  • YAG Ceramics is a bulk material obtained by adding dopants (Nd, Yb, Cr, Sm, Er, etc.) to a polycrystal based on Y 3 Al 5 O 12 for laser oscillation or light absorption. Further, there is no absorption by the doping element, and the transmittance from the visible light region (wavelength 380 nm to 760 nm) to the vicinity of the infrared region (upper limit is 3000 nm wavelength) is 80% or more.
  • the refractive index of YAG ceramics varies slightly depending on the type of dopant, but is about 1.83 with respect to light having a wavelength of 650 nm. It is preferable to use a high-density material with a small amount of residual pores in the bulk, and depending on the purpose, additive-free YAG ceramics may be used.
  • the optical glass can absorb the light oscillated from the YAG ceramics and can be used as a light absorption layer (clad) for reducing parasitic oscillation. It has a refractive index (refractive index of 1.71 to 1.91 for light with a wavelength of 650 nm) and a thermal expansion rate (7 to 9 ppm / K) equivalent to those of YAG ceramics forming a laser medium (core), and oscillates YAG. It is preferable to use a material having light absorption at a wavelength (wavelength 1030 nm, 1064 nm).
  • a method for producing a YAG ceramics bonded body In order to join YAG ceramics and YAG ceramics or optical glass, the surface of one YAG ceramic is coated with molten glass (adhesive glass), and then the other YAG ceramic or optical glass is laminated on the coated surface, and then By slowly cooling, a YAG ceramics bonded body via glass can be produced as a bonding layer as shown in FIG. Further, by using a material of the same quality as the optical glass (such as titanosilicate glass) as the adhesive glass, a bonded body substantially made of YAG ceramics / optical glass can be produced.
  • a material of the same quality as the optical glass such as titanosilicate glass
  • the YAG ceramics bonded body bonded via glass as the bonding layer can be used, for example, in the following laser applications.
  • a schematic diagram of a standard laser application is shown in FIG.
  • the laser medium 3 (Yb: YAG ceramics, etc.), which is a phosphor, is excited by the excitation light 2 of the laser diode 1, and the light is amplified in a resonator sandwiched between the opposing high-reflection mirrors 4 and 4', and then the laser 5 is used. Release as. At this time, the end surface of the laser medium 3 becomes a reflecting surface, and parasitic oscillation 6 that oscillates the laser in a direction different from the surface formed by the mirrors 4 and 4'is generated. When this parasitic oscillation 6 occurs, the output is lower than the laser light predicted from the resonator composed of the original opposed mirrors 4 and 4', and it is required to reduce this.
  • a light absorption layer 7 having an equivalent refractive index and absorbing light in the oscillation wavelength band of the laser medium is formed around the laser medium.
  • Parasitic oscillation 6 can be prevented by bonding Cr: YAG ceramics doped with a transition metal such as Cr as the light absorption layer 7.
  • the applicant previously had an absorption coefficient of 0.1 to 10.0 cm -1 as the light absorption layer, the difference in refractive index from the laser medium was within ⁇ 0.1, and linear thermal expansion with the laser medium. It has been proposed to use glass (optical glass) having a coefficient difference of ⁇ 1 ppm / K or less (Japanese Patent Application No. 2019-002307).
  • a bonded body of YAG ceramics using the glass according to the present invention as a bonding layer, or a YAG ceramic Bonds with other optical materials can be applied.
  • the bonding between YAG ceramics as a laser medium and YAG ceramics or optical glass as a light absorption layer has been described, but for purposes other than bonding with the light absorption layer, for example, YAG ceramics as a laser medium.
  • the present invention can also be applied when a plurality of YAG ceramics of the same quality are bonded via a glass bonding layer for the purpose of increasing the diameter.
  • Example 1 Two 0.5 at% Yb: YAG (2 cm ⁇ 1 cm, 5 mm thick) were prepared as YAG ceramics, and a glass material (LX-57B: manufactured by Nippon Electric Glass Co., Ltd.) was prepared as a bonding layer. The glass material was melted at 1000 ° C., the molten glass was coated on the surface of one YAG ceramic, and then the other YAG ceramic was laminated to prepare a YAG ceramic joint.
  • the refractive index of Yb: YAG ceramics is 1.83 with respect to light having a wavelength of 650 nm, and the refractive index of the glass material of the bonding layer is 1.71 with respect to the same wavelength.
  • the coefficient of thermal expansion of Yb: YAG ceramics is 8 ppm / K, and the coefficient of thermal expansion of the glass material is 8 ppm / K.
  • Laser light (wavelength: 650 nm) was incident on the YAG ceramic base material (before joining) and the obtained YAG ceramic bonded body (after joining), and the transmittance before and after joining was measured and compared. The rate was 7%, and it was confirmed that the light reflection at the junction interface was suppressed. Further, it was confirmed that peeling, cracking, etc. did not occur in this bonded body even in a high temperature environment of 600 ° C. or higher above the glass transition point and in a low temperature environment of liquid nitrogen temperature.
  • Example 2 Prepare 0.5 at% Yb: YAG (2 cm x 1 cm, 5 mm thick) and titanosilicate glass (optical glass: 2 cm x 1 cm, 5 mm thick) as YAG ceramics, and use the same glass material as the optical glass as the bonding layer.
  • the glass material was melted at 1250 ° C., the molten glass was coated on the surface of YAG ceramics, and then optical glass was laminated to prepare a YAG ceramics joint.
  • the refractive index of the optical glass is 1.81 with respect to light having a wavelength of 650 nm, and the coefficient of thermal expansion is 7 ppm / K.
  • Laser light (wavelength: 650 nm) was incident on the YAG ceramic base material (before joining) and the obtained YAG ceramic bonded body (after joining), and the transmittances before and after joining were compared. It was 1.5%, and it was confirmed that the light reflection at the junction interface was suppressed. Further, it was confirmed that peeling, cracking, etc. did not occur in this bonded body even in a high temperature environment of 700 ° C. or higher above the glass transition point and in a low temperature environment of liquid nitrogen temperature.
  • the present invention provides a bonded body of YAG ceramics and YAG ceramics, or a bonded body of YAG ceramics and optical glass, in which light reflection at the bonding interface is suppressed and destruction is unlikely to occur even with a temperature change. It has the excellent effect of being able to.
  • the ceramic joint according to the present invention is useful as a laser application such as a high power laser (amplifier).
  • Laser diode 2 Excitation light 3 Laser medium (core) 4 Mirror 5 Laser 6 Parasitic oscillation 7 Light absorption layer (clad)

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  • Electromagnetism (AREA)
  • Physics & Mathematics (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical & Material Sciences (AREA)
  • Optics & Photonics (AREA)
  • Plasma & Fusion (AREA)
  • Ceramic Engineering (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Materials Engineering (AREA)
  • Structural Engineering (AREA)
  • Organic Chemistry (AREA)
  • Lasers (AREA)
  • Ceramic Products (AREA)
  • Laser Beam Processing (AREA)
  • Joining Of Glass To Other Materials (AREA)
PCT/JP2020/038554 2020-02-07 2020-10-13 Ｙａｇセラミックス接合体及びその製造方法 Ceased WO2021157135A1 (ja)

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EP20917282.4A EP4023621A4 (en) 2020-02-07 2020-10-13 JAG YAG CERAMIC BODY AND METHOD FOR PRODUCING SAME
US17/763,451 US12160081B2 (en) 2020-02-07 2020-10-13 YAG ceramic joined body and production method therefor
JP2021575609A JP7503579B2 (ja) 2020-02-07 2020-10-13 Ｙａｇセラミックス接合体及びその製造方法
CN202080069254.2A CN114502520B (zh) 2020-02-07 2020-10-13 Yag陶瓷接合体及其制造方法
JP2022206720A JP2023029447A (ja) 2020-02-07 2022-12-23 Ｙａｇセラミックス接合体及びその製造方法

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US20220393424A1 (en) 2022-12-08
JPWO2021157135A1 (https=) 2021-08-12
JP2023029447A (ja) 2023-03-03
JP7503579B2 (ja) 2024-06-20
CN114502520A (zh) 2022-05-13

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