WO2021107049A1 - Électrode d'ionisation et élément de saphir - Google Patents

Électrode d'ionisation et élément de saphir Download PDF

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Publication number
WO2021107049A1
WO2021107049A1 PCT/JP2020/044103 JP2020044103W WO2021107049A1 WO 2021107049 A1 WO2021107049 A1 WO 2021107049A1 JP 2020044103 W JP2020044103 W JP 2020044103W WO 2021107049 A1 WO2021107049 A1 WO 2021107049A1
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WO
WIPO (PCT)
Prior art keywords
tube
sapphire
electrode
peripheral surface
axial direction
Prior art date
Application number
PCT/JP2020/044103
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English (en)
Japanese (ja)
Inventor
善則 久保
一郎 坂野
Original Assignee
京セラ株式会社
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Filing date
Publication date
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Publication of WO2021107049A1 publication Critical patent/WO2021107049A1/fr

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    • C—CHEMISTRY; METALLURGY
    • C30—CRYSTAL GROWTH
    • C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
    • C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
    • C30B29/10—Inorganic compounds or compositions
    • C30B29/16—Oxides
    • C30B29/20—Aluminium oxides
    • 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
    • H01S3/02—Constructional details
    • H01S3/03—Constructional details of gas laser discharge tubes
    • H01S3/038—Electrodes, e.g. special shape, configuration or composition
    • 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
    • H01S3/09—Processes or apparatus for excitation, e.g. pumping
    • H01S3/097—Processes or apparatus for excitation, e.g. pumping by gas discharge of a gas laser
    • H01S3/0977—Processes or apparatus for excitation, e.g. pumping by gas discharge of a gas laser having auxiliary ionisation means
    • 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
    • H01S3/22—Gases
    • H01S3/223—Gases the active gas being polyatomic, i.e. containing two or more atoms
    • H01S3/225—Gases the active gas being polyatomic, i.e. containing two or more atoms comprising an excimer or exciplex

Definitions

  • the present disclosure relates to an ionization electrode and a sapphire member used in an excimer laser device or the like.
  • An excimer laser is a laser that uses an excimer.
  • a mixed gas containing a halogen gas and a rare gas is sealed and discharged, an excited rare gas / halogen dimer (excimer) is generated, and energy is generated when the gas is transferred to the base state rare gas and halogen. Is converted into light and emitted.
  • a continuous laser can be obtained by continuously repeating the discharge.
  • the laser wavelength obtained varies depending on the combination of the enclosed gas, and ArF excimer laser (wavelength 193 nm), KrF excimer laser (wavelength 248 nm), XeCl excimer laser (wavelength 308 nm), XeF excimer laser (wavelength 351 nm), etc.
  • ArF excimer laser wavelength 193 nm
  • KrF excimer laser wavelength 248 nm
  • XeCl excimer laser wavelength 308 nm
  • XeF excimer laser wavelength 351 nm
  • preliminary ionization is performed in order to obtain a stable laser excitation discharge. This is because the laser gas is ionized in advance.
  • a first electrode and a second electrode are arranged inside and outside the tube which is an insulator, respectively, and a voltage is applied between these electrodes to generate a corona discharge.
  • Patent Document 1 describes the use of polycrystalline or single crystal alumina as the tube.
  • the tube used for such a preliminary ionization electrode is required to have good corrosion resistance and discharge characteristics because it is discharged in an atmosphere of a corrosive gas such as a halogen gas. Further, in order to insert the first electrode and to cause an appropriate corona discharge as a preliminary ionization, the tube is required to have little deformation and excellent mechanical strength.
  • the first ionization electrode of the present disclosure is used in a device using a corrosive gas, and is a tube made of sapphire, a first electrode inserted inside the tube, and the outside of the tube.
  • the tube is provided with a second electrode arranged in the tube, and the axial direction of the tube is substantially parallel to the c-axis direction of the sapphire.
  • the second ionizing electrode of the present disclosure is used in a device using a corrosive gas, and is a tube made of sapphire, a first electrode inserted inside the tube, and the outside of the tube.
  • the second electrode is provided with a second electrode arranged in, and the axial direction of the tube is substantially perpendicular to the c-axis direction of the sapphire, and the second electrode is substantially parallel to the c-axis of the sapphire when viewed from the axial center of the tube. Have been placed.
  • the sapphire member of the present disclosure has a tube shape used in an apparatus using a corrosive gas, has an inner peripheral surface and an outer peripheral surface extending in the axial direction, and is deep from the inner peripheral surface and the outer peripheral surface, respectively. There is no processed alteration layer in the region within 0.5 mm, and there are bubbles arranged in a streak in the axial direction.
  • FIG. 2A It is explanatory drawing which shows the use example of the ionization electrode of this disclosure in an excimer laser apparatus. It is the schematic sectional drawing which shows one Embodiment of the ionization electrode of this disclosure. It is a schematic perspective view of the ionization electrode shown in FIG. 2A. It is a top view which shows an example of the mold used for manufacturing the tube made of sapphire. It is a partial top view of the AA'line of FIG. It is a micrograph which shows an example of the streak bubble which the sapphire member of this disclosure has
  • FIG. 1 is an explanatory view showing an example of use of the ionization electrode of the present disclosure in an excimer laser apparatus
  • FIGS. 2A and 2B are a schematic cross-sectional view and a schematic perspective view showing an embodiment of the ionization electrode shown in FIG. Is.
  • the ionization electrode may be referred to as a preliminary ionization electrode.
  • the excimer laser apparatus includes a chamber 100 in which a mixed gas containing a halogen gas and a rare gas, which are corrosive gases, is sealed.
  • a mixed gas containing a halogen gas and a rare gas, which are corrosive gases is sealed.
  • the halogen gas include fluorine (F 2 ) gas
  • the rare gas include argon (Ar) gas and krypton (Kr) gas.
  • an anode 101 for oscillating a laser beam and a cathode 102 are arranged to face each other as main electrodes.
  • the anode 101 and the cathode 102 each extend long in the vertical direction of the paper surface and are connected to the high voltage pole and the ground pole (neither shown) of the pulse voltage source 103.
  • the ground electrode is connected to, for example, chamber 100.
  • a preliminary ionization electrode 10 is provided in the chamber 100.
  • the preliminary ionization electrode 10 stabilizes the pulse discharge P by causing a discharge called preliminary ionization in which the mixed gas is ionized prior to the pulse discharge P.
  • the preliminary ionization electrode 10 includes a tube 3 made of insulating sapphire (hereinafter, may be referred to as sapphire tube 3) and a first electrode inserted inside the sapphire tube 3. 1 and a second electrode 2 arranged outside the sapphire tube 3 are provided.
  • the first electrode 1 is formed of a round bar-shaped conductor.
  • the second electrode 2 is formed of a plate-shaped conductor.
  • the first electrode 1 is connected to the ground electrode of the pulse voltage source 103.
  • the sapphire tube 3 is arranged parallel to the longitudinal direction of the main electrode.
  • the sapphire tube 3 shown in FIG. 2B has both ends open, but one end may be sealed. Further, the light emission due to the preliminary ionization discharge may be generated on the inner peripheral surface 3a side of the shear tube 3 or on the outer peripheral surface 3b side. Since the sapphire tube 3 is transparent, the light generated on the inner peripheral surface 3a side can be transmitted.
  • Sapphire alumina single crystal
  • various physical properties such as coefficient of thermal expansion, permittivity, and refractive index are different in the direction perpendicular to the c-axis and the direction parallel to the c-axis. .. Therefore, it may be deformed due to expansion and contraction due to a temperature change, the state of the potential may differ depending on the direction in which the voltage is applied, and the speed and refraction may differ depending on the traveling direction of light.
  • the axial direction of the sapphire tube 3, that is, the direction of the arrow B in FIG. 2B is substantially parallel to the c-axis direction of the sapphire.
  • substantially parallel to the c-axis direction means that in addition to being completely parallel, an angle deviation of about ⁇ 10 ° from the parallel direction is allowed.
  • the thickness of the sapphire tube 3 is preferably 0.5 mm or more and 10 mm or less, preferably 1 mm or more and 5 mm or less.
  • the outer diameter of the sapphire tube 3 is preferably 1 mm or more and 50 mm or less, preferably 2 mm or more and 25 mm or less.
  • the total length of the sapphire tube 3 is 500 mm or more, and the straightness of the outer peripheral surface is 1.0 mm or less, preferably 0.5 mm or less. This facilitates the insertion of the first electrode 1 into the sapphire tube 3. Straightness can be measured, for example, by the following method.
  • Two V-shaped blocks conforming to JIS B7540 are arranged on the surface plate, and both ends of the tube 3 are supported by V-planes.
  • the tube 3 is rotated once on the V surface, and the distance from the reference line at the position where the outer peripheral surface 3b is farthest from the reference line connecting both ends is measured using a microgauge or the like to obtain straightness.
  • the surface of the sapphire tube 3 is preferably smooth in terms of corrosion resistance.
  • the surface roughness (arithmetic mean roughness) Sa on the inner and outer peripheral surfaces of the sapphire tube 3 is preferably 1.0 ⁇ m or less, preferably 0.2 ⁇ m or less.
  • the surface roughness Sa can be measured according to ISO25178, for example, using a laser microscope with a measurement area of 500 ⁇ m ⁇ .
  • the sapphire tube 3 can be produced by using the EFG method (edge defined film fed growth method) known as a method for growing a single crystal.
  • EFG method edge defined film fed growth method
  • the raw material of the single crystal filled in the crucible is heated and melted, and the seed crystal is formed in the sapphire melt raised to the upper surface of the mold by utilizing the capillary phenomenon by the slit in the mold installed in the crucible.
  • a single crystal having a predetermined shape is grown by bringing the (seed) into contact with the seed and pulling it upward.
  • FIG. 3 is a schematic view of the mold 4 used for manufacturing the sapphire tube 3 as a top view
  • FIG. 4 is a cross-sectional view taken along the line AA'.
  • the mold 4 includes an annular outer mold 4a on the outer peripheral side and an inner mold 4b arranged inside the annular outer mold 4a.
  • an annular slit 5 exists between the annular outer mold 4a and the inner mold 4b.
  • the lower end of the slit 5 is immersed in the melt existing in the lower part of the mold 4, and has a function of supplying the melt to the opening 6 of the slit 5 by a capillary phenomenon. Therefore, the melt is present in the opening 6.
  • a crystal growing surface 7 is arranged on the upper surface of the mold 4 so as to surround the opening 6, and a recess 9 is formed on the upper surface of the mold 4 at a position corresponding to a through hole of the sapphire tube 3. ing.
  • the crystal growth region 8 is a portion of the upper surface of the mold 4 excluding the recess 9, that is, a region where the opening 6 of the slit 5 and the crystal growth surface 7 are combined.
  • the crystal growth surface 7 is inclined so as to be lower toward the slit 5, but it may be a horizontal surface.
  • the sapphire melt rises through the slit 5, reaches the opening 6, and extends to the crystal growth surface 7. That is, the sapphire melt exists on the crystal growth region 8.
  • the seed crystal can be brought into contact with the sapphire melt, and then the seed crystal can be produced as a sapphire tube 3 that substantially coincides with the crystal growth region 8.
  • the sapphire melt can be obtained by heating and melting a sapphire raw material composed of alumina powder at a temperature equal to or higher than the melting point of alumina, for example, 2080 ° C.
  • the cross-sectional shape of the seed crystal may be substantially the same as that of the crystal growth region 8. Seed crystals can be prepared by processing sapphire lumps.
  • the seed crystal is made of sapphire, and the pulling direction is the c-axis.
  • the obtained sapphire tube 3 has an axial direction substantially parallel to the c-axis of the sapphire.
  • the obtained tubular sapphire member has relatively uniform (isotropic) physical properties in the thickness direction, is less deformed due to thermal expansion, has a relatively uniform dielectric constant, and has a uniform discharge. Therefore, the obtained tubular sapphire member is suitable as the sapphire tube 3 in the excimer laser apparatus. It can be confirmed by measuring the crystal orientation using the X-ray diffraction method that the axial direction of the tube 3 is substantially parallel to the c-axis of sapphire.
  • the sapphire member used as the sapphire tube 3 has an inner peripheral surface 3a and an outer peripheral surface 3b extending in the axial direction, and has a depth of 0. There is no processed alteration layer in the region within 5 mm, and the bubbles are arranged in a streak pattern in the axial direction.
  • a work-altered layer can be defined as a layer in which crystal defects such as microcracks and dislocations are introduced into the crystal surface by mechanical processing such as cutting, grinding, and polishing. Specifically, it is more than a bulk portion. Refers to a surface layer with many microcracks, dislocations, etc. (for example, 10 times or more).
  • the corrosion resistance is lowered and particles are likely to be generated.
  • the processed altered layer exists in a region having a depth of 0.5 mm or less can be confirmed by, for example, optical microscope observation, CL (cathodoluminescence) observation, and TEM (transmission electron microscope) observation.
  • CL cathodoluminescence
  • TEM transmission electron microscope
  • the sapphire member has bubbles arranged in a streak pattern in the axial direction of the tube 3 in regions within 0.5 mm in depth from the inner peripheral surface 3a and the outer peripheral surface 3b, respectively.
  • FIG. 5 shows an example of streaky bubbles generated on the outer peripheral surface of the sapphire tube 3.
  • the streaky bubbles can absorb and mitigate the impact of the mechanical impact, thermal impact, etc. on the sapphire tube 3 and stop the expansion of cracks.
  • the streaky bubbles determine the growing conditions (pulling speed, atmosphere, growing temperature, etc.) when pulling the tube 3 from the surface of the mold 4 and the configuration and shape of the growing device (shape, inclination angle, etc. of the crystal growing surface 7). It can be generated (or the status of occurrence is controlled) by adjusting.
  • the streaky bubbles have a diameter of, for example, about 5 ⁇ m to 40 ⁇ m, and one to several streaky bubbles are arranged in the circumferential direction of the tube 3 and arranged in a streak shape in the axial direction.
  • the width of one muscle is, for example, 300 ⁇ m or less, and a plurality of muscles are arranged in the circumferential direction of the tube 3.
  • the pitch between the muscles is, for example, about 0.3 mm to 2 mm.
  • the density of bubbles per unit area as seen from the outer peripheral surface or the inner peripheral surface is 250 to 2500 cells / mm 2 .
  • the density of bubbles is determined, for example, by measuring the number of bubbles 1b in the region containing the streaky bubbles 1b and dividing by the area of the measurement area.
  • the ionization electrode (second ionization electrode) according to another embodiment of the present disclosure will be described.
  • the difference between the second ionizing electrode and the first ionizing electrode described above is that the c-axis of the sapphire is substantially parallel to the arrow A in FIG. 2A, and the axial direction of the sapphire tube 3, that is, FIG. 2B.
  • the direction of the arrow B is substantially perpendicular to the c-axis direction of the sapphire
  • the second electrode 2 is located in the direction substantially parallel to the c-axis of the sapphire when viewed from the axis of the tube 3, that is, in the direction of the arrow A in FIG. 2A. It is the same as the first ionizing electrode except that it is arranged.
  • being substantially perpendicular to the c-axis direction of sapphire means that in addition to being completely vertical, a deviation of about ⁇ 10 ° from the vertical direction is allowed.
  • the direction substantially parallel to the c-axis of sapphire means that in addition to being completely parallel, a deviation of about ⁇ 10 ° from the parallel direction is allowed.
  • the dielectric constant of sapphire is high in the c-axis direction, electrolysis in a gas containing a corrosive gas becomes strong, and it becomes easy to discharge.
  • the c-axis of the seed crystal is arranged so as to be substantially perpendicular to the pulling direction, and in that state.
  • the sapphire melt may be pulled up. It can be confirmed by the crystal orientation measurement using the X-ray diffraction method that the axial direction of the sapphire tube 3 is substantially perpendicular to the c-axis of the sapphire.
  • the sapphire member used in the second ionization electrode according to the present embodiment also has no processing alteration layer in the regions within 0.5 mm in depth from the inner peripheral surface 3a and the outer peripheral surface 3b, respectively, and is in the axial direction. It has bubbles arranged in a streak pattern.
  • the first and second ionization electrodes of the present disclosure both include a tube made of sapphire, there is little deformation, and corrosion resistance and mechanical strength are good. Therefore, the first and second ionization electrodes are suitable for use as preliminary ionization electrodes for devices that use corrosive gases, such as excimer laser devices.
  • the sapphire member of the present disclosure has a tube shape, and since there is no processed alteration layer on each surface region of the inner peripheral surface and the outer peripheral surface thereof, it has high corrosion resistance and has muscular bubbles arranged in a streak shape in the axial direction. Therefore, it also has the effect of absorbing and mitigating the impact and stopping the growth of cracks.
  • the sapphire member of the present disclosure can be used not only as an ionization electrode, but also as a protective tube for a long member (for example, a thermocouple, etc.), a flow path member, a dielectric member for electric discharge, an insulating member, and the like. It can be widely used in various plasma processing devices, etching devices, film forming devices, excimer laser devices, and the like.

Abstract

L'invention concerne une électrode d'ionisation, est utilisée pour un dispositif utilisant un gaz corrosif, qui comprend : un tube composé de saphir ; une première électrode insérée dans le tube ; et une seconde électrode disposée à l'extérieur du tube, la direction axiale du tube étant sensiblement parallèle à une direction de l'axe c du saphir ou étant sensiblement perpendiculaire à la direction de l'axe c du saphir ; et, vu depuis le centre axial du tube, la seconde électrode est disposée dans une direction sensiblement parallèle à l'axe c du saphir.
PCT/JP2020/044103 2019-11-27 2020-11-26 Électrode d'ionisation et élément de saphir WO2021107049A1 (fr)

Applications Claiming Priority (2)

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JP2019-214527 2019-11-27
JP2019214527 2019-11-27

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Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS51102379A (ja) * 1975-03-07 1976-09-09 Hitachi Ltd Hodento
JP2000236128A (ja) * 1999-02-10 2000-08-29 Lambda Physik G Zur Herstellung Von Lasern Mbh ガスレーザ用の前期イオン化装置
US20110275546A1 (en) * 2008-12-12 2011-11-10 Instituto Mexicano Del Petroleo Foaming composition for high temperature and salinity
WO2018181981A1 (fr) * 2017-03-30 2018-10-04 京セラ株式会社 Élément de saphir tubulaire, échangeur de chaleur, dispositif de fabrication de semi-conducteurs et procédé destiné à fabriquer un élément de saphir tubulaire

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS51102379A (ja) * 1975-03-07 1976-09-09 Hitachi Ltd Hodento
JP2000236128A (ja) * 1999-02-10 2000-08-29 Lambda Physik G Zur Herstellung Von Lasern Mbh ガスレーザ用の前期イオン化装置
US20110275546A1 (en) * 2008-12-12 2011-11-10 Instituto Mexicano Del Petroleo Foaming composition for high temperature and salinity
WO2018181981A1 (fr) * 2017-03-30 2018-10-04 京セラ株式会社 Élément de saphir tubulaire, échangeur de chaleur, dispositif de fabrication de semi-conducteurs et procédé destiné à fabriquer un élément de saphir tubulaire

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