US20210226105A1 - Silica glass member for hermetic sealing of ultraviolet smd led element and method for manufacturing quartz glass member for ultraviolet led - Google Patents

Silica glass member for hermetic sealing of ultraviolet smd led element and method for manufacturing quartz glass member for ultraviolet led Download PDF

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Publication number
US20210226105A1
US20210226105A1 US16/306,185 US201716306185A US2021226105A1 US 20210226105 A1 US20210226105 A1 US 20210226105A1 US 201716306185 A US201716306185 A US 201716306185A US 2021226105 A1 US2021226105 A1 US 2021226105A1
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Prior art keywords
silica glass
glass member
hermetic sealing
ultraviolet
silica
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Abandoned
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US16/306,185
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English (en)
Inventor
Akira Fujinoki
Hiroyuki Nishimura
Akira Sato
Yuya YOKOSAWA
Tatsuya Mori
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Shin Etsu Quartz Products Co Ltd
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Shin Etsu Quartz Products Co Ltd
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Filing date
Publication date
Priority claimed from JP2016110033A external-priority patent/JP2017216389A/ja
Priority claimed from JP2016131887A external-priority patent/JP6789011B2/ja
Application filed by Shin Etsu Quartz Products Co Ltd filed Critical Shin Etsu Quartz Products Co Ltd
Assigned to SHIN-ETSU QUARTZ PRODUCTS CO., LTD. reassignment SHIN-ETSU QUARTZ PRODUCTS CO., LTD. ASSIGNMENT OF ASSIGNORS INTEREST (SEE DOCUMENT FOR DETAILS). Assignors: SATO, AKIRA, YOKOSAWA, YUYA, FUJINOKI, AKIRA, MORI, TATSUYA, NISHIMURA, HIROYUKI
Publication of US20210226105A1 publication Critical patent/US20210226105A1/en
Abandoned legal-status Critical Current

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    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
    • C03B20/00—Processes specially adapted for the production of quartz or fused silica articles, not otherwise provided for
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L33/00—Semiconductor devices having potential barriers specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
    • H01L33/48—Semiconductor devices having potential barriers specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof characterised by the semiconductor body packages
    • H01L33/58—Optical field-shaping elements
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
    • C03B19/00—Other methods of shaping glass
    • C03B19/06—Other methods of shaping glass by sintering, e.g. by cold isostatic pressing of powders and subsequent sintering, by hot pressing of powders, by sintering slurries or dispersions not undergoing a liquid phase reaction
    • C03B19/066—Other methods of shaping glass by sintering, e.g. by cold isostatic pressing of powders and subsequent sintering, by hot pressing of powders, by sintering slurries or dispersions not undergoing a liquid phase reaction for the production of quartz or fused silica articles
    • 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
    • C03C3/04—Glass compositions containing silica
    • C03C3/06—Glass compositions containing silica with more than 90% silica by weight, e.g. quartz
    • 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
    • C03C4/0085—Compositions for glass with special properties for UV-transmitting glass
    • G—PHYSICS
    • G02—OPTICS
    • G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
    • G02B19/00—Condensers, e.g. light collectors or similar non-imaging optics
    • G02B19/0033—Condensers, e.g. light collectors or similar non-imaging optics characterised by the use
    • G02B19/0047—Condensers, e.g. light collectors or similar non-imaging optics characterised by the use for use with a light source
    • G02B19/0061—Condensers, e.g. light collectors or similar non-imaging optics characterised by the use for use with a light source the light source comprising a LED
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L33/00—Semiconductor devices having potential barriers specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
    • H01L33/48—Semiconductor devices having potential barriers specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof characterised by the semiconductor body packages
    • H01L33/483—Containers
    • H01L33/486—Containers adapted for surface mounting
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L33/00—Semiconductor devices having potential barriers specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
    • H01L33/48—Semiconductor devices having potential barriers specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof characterised by the semiconductor body packages
    • H01L33/52—Encapsulations
    • H01L33/56—Materials, e.g. epoxy or silicone resin
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
    • C03B2201/00—Type of glass produced
    • C03B2201/02—Pure silica glass, e.g. pure fused quartz
    • C03B2201/03—Impurity concentration specified
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
    • C03B2201/00—Type of glass produced
    • C03B2201/02—Pure silica glass, e.g. pure fused quartz
    • C03B2201/03—Impurity concentration specified
    • C03B2201/04—Hydroxyl ion (OH)
    • 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
    • C03C2201/00—Glass compositions
    • C03C2201/02—Pure silica glass, e.g. pure fused quartz
    • 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
    • C03C2201/00—Glass compositions
    • C03C2201/06—Doped silica-based glasses
    • C03C2201/20—Doped silica-based glasses containing non-metals other than boron or halide
    • C03C2201/23—Doped silica-based glasses containing non-metals other than boron or halide containing hydroxyl groups
    • 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
    • C03C2201/00—Glass compositions
    • C03C2201/80—Glass compositions containing bubbles or microbubbles, e.g. opaque quartz glass
    • 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
    • C03C2203/00—Production processes
    • C03C2203/50—After-treatment
    • C03C2203/52—Heat-treatment
    • C03C2203/54—Heat-treatment in a dopant containing atmosphere
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F21—LIGHTING
    • F21V—FUNCTIONAL FEATURES OR DETAILS OF LIGHTING DEVICES OR SYSTEMS THEREOF; STRUCTURAL COMBINATIONS OF LIGHTING DEVICES WITH OTHER ARTICLES, NOT OTHERWISE PROVIDED FOR
    • F21V5/00—Refractors for light sources
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F21—LIGHTING
    • F21V—FUNCTIONAL FEATURES OR DETAILS OF LIGHTING DEVICES OR SYSTEMS THEREOF; STRUCTURAL COMBINATIONS OF LIGHTING DEVICES WITH OTHER ARTICLES, NOT OTHERWISE PROVIDED FOR
    • F21V5/00—Refractors for light sources
    • F21V5/007—Array of lenses or refractors for a cluster of light sources, e.g. for arrangement of multiple light sources in one plane
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F21—LIGHTING
    • F21Y—INDEXING SCHEME ASSOCIATED WITH SUBCLASSES F21K, F21L, F21S and F21V, RELATING TO THE FORM OR THE KIND OF THE LIGHT SOURCES OR OF THE COLOUR OF THE LIGHT EMITTED
    • F21Y2115/00—Light-generating elements of semiconductor light sources
    • F21Y2115/10—Light-emitting diodes [LED]
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L25/00—Assemblies consisting of a plurality of individual semiconductor or other solid state devices ; Multistep manufacturing processes thereof
    • H01L25/03—Assemblies consisting of a plurality of individual semiconductor or other solid state devices ; Multistep manufacturing processes thereof all the devices being of a type provided for in the same subgroup of groups H01L27/00 - H01L33/00, or in a single subclass of H10K, H10N, e.g. assemblies of rectifier diodes
    • H01L25/04—Assemblies consisting of a plurality of individual semiconductor or other solid state devices ; Multistep manufacturing processes thereof all the devices being of a type provided for in the same subgroup of groups H01L27/00 - H01L33/00, or in a single subclass of H10K, H10N, e.g. assemblies of rectifier diodes the devices not having separate containers
    • H01L25/075—Assemblies consisting of a plurality of individual semiconductor or other solid state devices ; Multistep manufacturing processes thereof all the devices being of a type provided for in the same subgroup of groups H01L27/00 - H01L33/00, or in a single subclass of H10K, H10N, e.g. assemblies of rectifier diodes the devices not having separate containers the devices being of a type provided for in group H01L33/00
    • H01L25/0753—Assemblies consisting of a plurality of individual semiconductor or other solid state devices ; Multistep manufacturing processes thereof all the devices being of a type provided for in the same subgroup of groups H01L27/00 - H01L33/00, or in a single subclass of H10K, H10N, e.g. assemblies of rectifier diodes the devices not having separate containers the devices being of a type provided for in group H01L33/00 the devices being arranged next to each other
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L2933/00—Details relating to devices covered by the group H01L33/00 but not provided for in its subgroups
    • H01L2933/0008—Processes
    • H01L2933/0033—Processes relating to semiconductor body packages
    • H01L2933/0058—Processes relating to semiconductor body packages relating to optical field-shaping elements
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L33/00—Semiconductor devices having potential barriers specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
    • H01L33/02—Semiconductor devices having potential barriers specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof characterised by the semiconductor bodies
    • H01L33/26—Materials of the light emitting region
    • H01L33/30—Materials of the light emitting region containing only elements of Group III and Group V of the Periodic Table
    • H01L33/32—Materials of the light emitting region containing only elements of Group III and Group V of the Periodic Table containing nitrogen

Definitions

  • the present invention firstly relates to a silica glass member to be used for hermetic sealing of an ultraviolet LED configured to emit ultraviolet light in a wavelength range of from 200 nm to 350 nm, and more specifically, to a silica glass member to be suitably used for hermetic sealing of, and as a transmission window material for, a surface mount-type package (commonly called a surface mount device (SMD)) having an ultraviolet LED mounted thereon and configured to emit ultraviolet light in a wavelength range of from 200 nm to 350 nm.
  • SMD surface mount device
  • the present invention secondly relates to a method of manufacturing a quartz glass member for an ultraviolet LED at a wavelength of from 200 nm to 400 nm.
  • An ultraviolet LED configured to emit light in a deep ultraviolet wavelength band is expected to be applied in a wide range of fields, such as virus sterilization, drinking water, air purification, resin curing, decomposition of environmental pollutants, a food field, and various kinds of medical equipment.
  • a gas light source such as a mercury lamp
  • a range of use of the gas light source is limited because of its short lifetime, its emission wavelength, which is limited only to an emission line of a gas, a substance contained therein that is harmful to a human body/environment, such as mercury, and an extremely large size and power consumption of the light source. Therefore, there has been an increasing demand for realization of an alternative technology. Under such circumstances, it is strongly desired to develop a mercury-free, low-environmental-load, downsized, high-output ultraviolet LED, and an ultraviolet LED using a nitride-based semiconductor (AlGaN) has been actively developed.
  • AlGaN nitride-based semiconductor
  • the ultraviolet LED emits light having a wavelength of from 200 nm to 400 nm, and has a problem in that a lens made of a silicone resin, which has hitherto been used for a visible light LED, undergoes deterioration of the resin or does not transmit the light.
  • Patent Documents 1 and 2 there is also a problem in that light extraction efficiency from an ultraviolet LED element is extremely low. Accordingly, a material that absorbs as little light as possible is required also for a window material or a lens material, and use of an optical member made of quartz glass has been considered (Patent Documents 1 and 2).
  • Patent Documents 9 and 11 an injection molding method is known as a method of manufacturing a quartz glass member with high accuracy in dimensions and shape.
  • This method can provide a transparent quartz glass body by degreasing and purifying a molded body, followed by firing, but has a problem in that purification treatment with chlorine or hydrogen chloride generates an optical absorption band at a wavelength of about 250 nm (5.0 eV) due to an oxygen-deficient defect (Non Patent Document 1).
  • Patent Documents 18 and 19 there is a proposal of a method involving, after vitrification, repairing the oxygen-deficient defect with an atmosphere containing oxygen or an atmosphere containing water vapor.
  • the method is limited in its effect to a quartz glass surface and requires treatment at high temperature. Accordingly, there is a risk of a reduction in transmittance due to an influence of contamination with an impurity (Patent Documents 18 and 19).
  • UVA ultraviolet light having a relatively long wavelength
  • UVA ultraviolet light having a relatively long wavelength
  • UVB (falling within a wavelength range of from 315 nm to 280 nm) and UVC (falling within a wavelength range of from 280 nm to 200 nm) each having a shorter wavelength than UVA are currently being intensively developed.
  • UV light having a wavelength of around 260 nm which is called a germicidal ray, has an intense germicidal action, and hence there is a demand that its practical use be soon achieved as inexpensive means for sterilizing water or sterilizing air.
  • UVA is formed on a sapphire substrate (Al 2 O 3 ), but UVB and UVC each require an AlN substrate due to lattice constant matching.
  • a window or a lens can be formed using an organic resin having a high UV transmission property, such as a silicone or Teflon (trademark).
  • an organic resin having a high UV transmission property such as a silicone or Teflon (trademark).
  • such organic material is insufficient in terms of light transmission property, and is also insufficient in terms of durability against UV light.
  • a borosilicate-based glass material having a satisfactory UV transmission property, which is often used for UVA, LED also cannot be used due to problems with the light transmission property (even borosilicate glass hardly transmits ultraviolet light having a wavelength of 350 nm or less) and the durability.
  • silica glass has been exclusively used as a window material or lens material for a UVB-LED or a UVC-LED (Patent Documents 1 and 2).
  • the silica glass has a high transmission property for UV light and also has high durability, and hence has sufficient characteristics as the window material or lens material for a UVB-LED or a UVC-LED.
  • the silica glass needs polishing in order to constitute a smooth surface having a high light transmission property suitable as the window material or the lens material, and hence cannot integrally constitute a smooth surface in a member in which a plain surface and a spherical surface coexist.
  • an outer peripheral portion has a plain surface and a structure having a convex spherical surface shape is formed inside a central side, a planar silica glass plate material and a hemispherical lens need to be each independently produced, polished, and bonded to each other.
  • LEDs not limited to ultraviolet LEDs
  • An LED element is an extremely fragile semiconductor element, and hence needs to be kept in a sealed environment for the purpose of preventing deterioration due to moisture or the like in the atmosphere.
  • the shell-type package is a package in which a surrounding space of an LED is sealed with a resin, and is widely used as an inexpensive LED package.
  • the SMD package has a structure in which an LED element is mounted on a concave recessed portion, a bottom surface and a side wall surface are each constituted of a reflector, and an upper surface is tightly sealed with a window material for hermetic sealing (Patent Document 3).
  • a first object of the present invention is to provide a silica glass member to be used for hermetic sealing of an ultraviolet LED configured to emit ultraviolet light in a wavelength range of from 200 nm or more to 350 nm or less, in particular, a silica glass member for hermetic sealing of an ultraviolet surface mount device (SMD) LED element to be suitably used for hermetic sealing of, and as a transmission window material for, a surface mount-type package (commonly called an SMD) having an ultraviolet LED mounted thereon and configured to emit ultraviolet light in a wavelength range of from 200 nm or more to 350 nm or less.
  • SMD ultraviolet surface mount device
  • a second object of the present invention is to provide a method of manufacturing a quartz glass member for an ultraviolet LED, which involves repairing an oxygen-deficient defect so that there can be obtained a quartz glass member for an ultraviolet LED improved in light absorption at a wavelength of about 250 nm and free of absorption due to a structural defect at a wavelength of from 200 nm to 400 nm.
  • a silica glass member for hermetic sealing of an ultraviolet SMD LED element that is configured to emit light in a wavelength range of from 250 nm to 350 nm and is placed in a hermetic sealing container having a container outer periphery joining plain surface formed in an outer peripheral portion thereof
  • the silica glass member for hermetic sealing including a silica glass substrate, which is homogeneously and integrally formed without an internal boundary, wherein the silica glass substrate has: a first surface on an inside opposed to the SMD LED element; and a second surface on an outside corresponding to the first surface, wherein an outer peripheral portion of the first surface has formed therein a substrate joining plain surface for joining to the container outer periphery joining plain surface, and wherein the second surface on the outside corresponding to the first surface has formed therein a lens-like convex portion configured to process emitted light from the ultraviolet SMD LED element.
  • a plurality of the lens-like convex portions are suitably formed on the second surface.
  • the substrate joining plain surface formed in the first surface preferably has a surface accuracy of 1 ⁇ m or less and a surface roughness of 0.1 ⁇ m or less in terms of Ra value, and the lens-like convex portion in the second surface preferably has a surface roughness of 0.2 ⁇ m or less in terms of Ra value.
  • the silica glass member for hermetic sealing of the present invention suitably has an internal transmittance at a thickness of 3 mm of 95% to 99% for ultraviolet light having a wavelength of 300 nm to 400 nm and an internal transmittance at a thickness of 3 mm of 92% to 99% or less for ultraviolet light having a wavelength of 245 nm or more and less than 300 nm.
  • bubbles contained in the silica glass member for hermetic sealing each preferably have a diameter of 50 ⁇ m or less, and the bubbles contained preferably have a total cross-sectional area of 1 ⁇ 10 ⁇ 3 mm 2 or less per 0.1 cm 3 of a volume of the silica glass member for hermetic sealing.
  • respective differences between internal transmittances of the silica glass member for hermetic sealing at a thickness of 3 mm for ultraviolet light having wavelengths of 350 nm, 300 nm, and 250 nm measured using an integrating sphere and internal transmittances thereof at a thickness of 3 mm for ultraviolet light having wavelengths of 350 nm, 300 nm, and 250 nm in general measurement are each suitably within 0.5%.
  • the silica glass member for hermetic sealing of the present invention preferably contains OH groups at a concentration of 0.1 ppm to 20 ppm.
  • the transmittance measurement with the integrating sphere is described.
  • a transmittance measurement apparatus based on a general optical system cannot distinguish between internal absorption and a scattering loss, and hence allows the scattering loss to be measured as absorption.
  • a transmittance measurement apparatus including the integrating sphere which is applicable to UV light, enables also scattered light to be introduced into a photodetector, and hence enables an absorption amount excluding the scattering loss to be measured.
  • an internal transmittance obtained by the transmittance measurement using the integrating sphere is considered not to include the scattering loss, and hence enables the scattering loss to be estimated through a comparison to an internal transmittance obtained by the general transmittance measurement.
  • the silica glass member for hermetic sealing of the present invention is silica glass suitable for a transparent window material and/or a lens material for an LED configured to emit ultraviolet light of UVB or UVC, in which the window material and the lens material, which have originally been separately cut out and subjected to polishing processing, are integrally formed, thereby having an advantage of being able to be inexpensively supplied.
  • the window material and the lens material which have originally been separately cut out and subjected to polishing processing, are integrally formed, thereby having an advantage of being able to be inexpensively supplied.
  • a plurality of lens portions are simultaneously formed in one silica glass member for sealing, there is an advantage in that a further cost effect is obtained.
  • silica glass molded body for hermetic sealing of the present invention having a complicated shape integrally and homogeneously formed into a predetermined shape can be obtained.
  • a window material or a lens material for ultraviolet light having a short wavelength such as UVB or UVC
  • mold molding using silica glass powder as a starting material. That is, the following are required in order to obtain the required transmittance, light durability, and moldability: the purity and particle size of the silica glass powder serving as the starting material be appropriately controlled; the inner surface finish of the molding mold be sufficiently smooth so as not to require post-polishing; structural defects of silica glass generated in the degreasing and molding steps be sufficiently suppressed/cured; and gaps between particles of the powder or a dissolved gas be sufficiently removed, to thereby reduce bubbles to prevent unnecessary scattered light from being emitted.
  • the integral molding of the silica member by the mold molding has a great advantage in terms of manufacturing method in that a plurality of lens portions can be simultaneously formed.
  • a plurality of lens portions can be simultaneously formed.
  • LED packages there have been an increasing number of packages each having placed therein a plurality of LEDs for the purpose of increasing the output. In this case, it is important that the positional relationship between individual LEDs and lens portions be accurately adjusted.
  • a window material and lens-like convex portions are manufactured in a state of being integrally formed, and as a result, the position of each of the lens portions is determined as a transfer of a position designed as a mold. Accordingly, there is an advantage in that the position can be extremely accurately determined.
  • the mold molding of a silica member besides the press molding, there are known injection molding, transfer molding, a slip casting method, and the like (Patent Documents 4 to 17).
  • a method of manufacturing a quartz glass member for an ultraviolet LED including: a molding step of mixing silica powder and a binder component, followed by molding the resultant mixture to obtain a molded body having a predetermined shape; a heat treatment step of subjecting the molded body to heating treatment with various gases; and a vitrification step of vitrifying the molded body subjected to heat treatment into transparent glass after the heat treatment step, wherein the heat treatment step includes: a degreasing step for organic matter at 1,000° C. or less with an atmosphere containing oxygen; a purification step for a metal impurity at 1,200° C.
  • the molding step suitably includes a molding step with a metal mold.
  • the oxidizing atmosphere suitably includes an atmosphere containing oxygen and/or water vapor.
  • the vitrification step is suitably performed at 1,700° C. or less.
  • the silica powder suitably contains at least one kind of spherical silica, and the silica powder suitably has an Al concentration of 70 ppm or less.
  • the method of manufacturing a quartz glass member for an ultraviolet LED suitably further includes performing heating treatment with a hydrogen atmosphere after the vitrification step.
  • the ultraviolet LED is suitably configured to emit ultraviolet light having a wavelength of from 200 nm to 400 nm.
  • the present invention exhibits the remarkable effect capable of providing the silica glass member to be used for hermetic sealing of an ultraviolet LED configured to emit ultraviolet light in a wavelength range of from 200 nm to 350 nm, in particular, the silica glass member for hermetic sealing of an ultraviolet SMD LED element to be suitably used for hermetic sealing of, and as a transmission window material for, a surface mount-type package (SMD) having an ultraviolet LED mounted thereon and configured to emit ultraviolet light in a wavelength range of from 200 nm or more to 350 nm or less.
  • SMD surface mount-type package
  • the present invention exhibits the remarkable effect capable of providing the method of manufacturing a quartz glass member for an ultraviolet LED, which involves repairing an oxygen-deficient defect so that there can be obtained a quartz glass member for an ultraviolet LED improved in light absorption at a wavelength of about 250 nm and free of absorption due to a structural defect at a wavelength of from 200 nm to 400 nm.
  • FIG. 1 is a cross-sectional explanatory view for illustrating a case one embodiment in which an ultraviolet SMD LED element is sealed with one embodiment of a silica glass member for hermetic sealing according to the present invention.
  • FIG. 2 is a planar explanatory view of the silica glass member for hermetic sealing illustrated in FIG. 1 .
  • FIG. 3 is a schematic perspective explanatory view of the silica glass member for hermetic sealing illustrated in FIG. 1 .
  • FIG. 4 is a cross-sectional explanatory view for illustrating another embodiment of a silica glass member for hermetic sealing according to the present invention.
  • FIG. 5 is a cross-sectional explanatory view for illustrating still another embodiment of a silica glass member for hermetic sealing according to the present invention.
  • FIG. 6 is a graph for showing the measurement results of the transmittance of a silica glass member produced in Example 1 together with the theoretical transmittance of silica glass.
  • FIG. 7 is a graph for showing the measurement results of the transmittance of the silica glass member produced in Example 1 obtained using an integrating sphere together with measurement results obtained by general measurement.
  • FIG. 8 is a graph for showing the measurement results of the transmittances of silica glass members produced using adhesives A to E in Comparative Example 1 together with the transmittance of the silica glass member of Example 1.
  • FIG. 9 is a graph for showing the transmittance measurement results of a quartz glass member for an ultraviolet LED obtained in Example 2 at wavelengths of from 200 nm to 400 nm.
  • FIG. 10 is a graph for showing transmittance measurement results of a quartz glass member obtained in Comparative Example 2 at wavelengths of from 200 nm to 400 nm.
  • FIG. 1 to FIG. 3 are explanatory diagrams for illustrating a case in which ultraviolet SMD LED elements 12 are sealed with one embodiment of a silica glass member 10 for hermetic sealing according to the present invention.
  • FIG. 1 is a cross-sectional explanatory diagram
  • FIG. 2 is a planar explanatory diagram
  • FIG. 3 is a schematic perspective explanatory diagram.
  • reference numeral 14 denotes a hermetic sealing container, which has a bottom wall 16 and a side wall 18 , and is configured to open upward through an opening 20 .
  • the upper surface of an upper end outer peripheral portion 22 of the side wall 18 of the hermetic sealing container 14 is formed to be a plain surface to serve as a container outer periphery joining plain surface 22 a .
  • the ultraviolet SMD LED elements 12 are placed on the upper surface of the bottom wall 16 . In the example illustrated in FIG. 1 and FIG. 2 , there is illustrated an example in which two ultraviolet SMD LED elements 12 are placed. However, two or more ultraviolet SMD LED elements 12 may be arranged, and for example, four or six ultraviolet SMD LED elements 12 may be arranged.
  • the silica glass member 10 for hermetic sealing of the present invention is not particularly limited in terms of dimensions as long as the opening 20 of the hermetic sealing container 14 can be sealed therewith.
  • the dimensions are set as follows: a width W of the silica glass member 10 for hermetic sealing illustrated in FIG. 2 : 3.5 mm, a length L of the silica glass member 10 for hermetic sealing illustrated in FIG. 2 : 7 mm, a diameter d of each of lens-like convex portions 28 illustrated in FIG. 2 : 3 mm, and a thickness t of a portion at a substrate joining plain surface 24 a illustrated in FIG. 1 : 1 mm.
  • the silica glass member 10 for hermetic sealing includes a silica glass substrate 10 A, which is homogeneously and integrally formed without an internal boundary, and is configured to emit light in a wavelength range of from 250 nm to 350 nm.
  • the silica glass substrate 10 A has a first surface 24 on an inside opposed to the SMD LED element 12 and a second surface 26 on an outside corresponding to the first surface 24 .
  • the outer peripheral portion of the first surface 24 has formed therein the substrate joining plain surface 24 a for joining to the container outer periphery joining plain surface 22 a .
  • the second surface 26 on the outside corresponding to the first surface 24 has formed therein the lens-like convex portions 28 configured to process emitted light from the ultraviolet SMD LED elements 12 .
  • FIG. 1 there is illustrated an example in which two lens-like convex portions 28 are formed in a parallel state with a connecting flat portion 30 interposed therebetween, corresponding to the two ultraviolet SMD LED elements 12 being placed in the hermetic sealing container 14 .
  • the hermetic sealing container 14 Under a state in which the container outer periphery joining plain surface 22 a of the hermetic sealing container 14 , in which the two ultraviolet SMD LED elements 12 are placed on the bottom wall 16 , and the substrate joining plain surface 24 a are joined to each other, the hermetic sealing container 14 is covered with the silica glass member 10 for hermetic sealing, to thereby bring the inside of the hermetic sealing container 14 into a hermetically sealed state.
  • the silica glass member 10 for hermetic sealing
  • the shape of the silica glass substrate 10 A may be as illustrated in FIG. 1 to FIG. 3 , in which the entirety of the first surface 24 is formed to be a plain surface and the second surface 26 has formed therein the lens-like convex portions 28 each having a hemispherical shape.
  • the shape of the silica glass substrate 10 A is not limited thereto, and any other shape may also be adopted as long as the shape can process emitted light from the ultraviolet SMD LED elements 12 .
  • FIG. 4 and FIG. 5 Examples of other shapes of the silica glass substrate 10 A are illustrated in FIG. 4 and FIG. 5 .
  • the two lens-like convex portions 28 are each formed in a hemispherical shape having formed therein a hollow portion 32 .
  • the lens-like convex portions 28 each having a hemispherical shape are formed in the second surface 26 as in FIG. 1 , while hanging enlarged portions 34 each having an ellipsoidal shape are formed in the first surface, corresponding to the two lens-like convex portions 28 each having a hemispherical shape.
  • the hermetic sealing container 14 in which the ultraviolet SMD LED elements 12 are placed is brought into a hermetically sealed state using the silica glass member 10 for hermetic sealing with the silica glass substrate 10 A having the shape of each of FIG. 4 and FIG. 5 , emitted light from the ultraviolet SMD LED elements 12 can be processed with satisfactory light extraction efficiency, as with the example of FIG. 1 to FIG. 3 .
  • a method of manufacturing a quartz glass member for an ultraviolet LED according to the present invention is described below.
  • an oxygen-deficient defect is generated by a chlorine-based gas to be used in purification treatment intended to remove a metal impurity, but heat treatment with an oxidizing atmosphere for repairing the oxygen-deficient defect is performed to repair the oxygen-deficient defect.
  • a quartz glass member for an ultraviolet LED improved in light absorption at a wavelength of about 250 nm and free of absorption due to a structural defect at a wavelength of from 200 nm to 400 nm.
  • An atmosphere containing oxygen and/or water vapor is suitably used as the oxidizing atmosphere.
  • quartz glass to be suitably used for an optical member for an ultraviolet LED can be obtained by the following method.
  • a molding step after mixing of silica powder and binder component, the raw materials subjected to kneading involving degassing treatment may be molded with a metal mold.
  • a heat treatment step the following steps are performed: a degreasing step at 1,000° C. or less with an atmosphere containing oxygen; a purification step for a metal impurity at 1,200° C. or less with an atmosphere containing hydrogen chloride; and a step of repairing an oxygen-deficient defect at a wavelength of about 250 nm at 1,150° C. or less with an oxidizing atmosphere.
  • a vitrification step after the heat treatment step is suitably performed at 1,700° C. or less.
  • An Al concentration in the silica powder serving as a main raw material is suitably 70 ppm or less. It is more preferred that heating treatment with a hydrogen atmosphere be performed after the vitrification step. With this, quartz glass to be suitably used for an optical member for an ultraviolet LED can be obtained.
  • the degassing treatment of the raw material has an effect of suppressing the generation of bubbles during the vitrification step.
  • binder component examples include cellulose-based components (methyl cellulose, carboxymethyl cellulose, and hydroxyethyl alcohol), agar, vinyl-based components (polyvinyl alcohol and polyvinyl pyrrolidone), starch-based components (dialdehyde starch, dextrin, and polylactic acid), acrylic components (sodium polyacrylate and methyl methacrylate), and a plant viscous substance.
  • cellulose-based components methyl cellulose, carboxymethyl cellulose, and hydroxyethyl alcohol
  • vinyl-based components polyvinyl alcohol and polyvinyl pyrrolidone
  • starch-based components dialdehyde starch, dextrin, and polylactic acid
  • acrylic components sodium polyacrylate and methyl methacrylate
  • a plant viscous substance examples include acrylic components (sodium polyacrylate and methyl methacrylate), and a plant viscous substance.
  • polyvinyl alcohol or methyl cellulose is suitable.
  • the degreasing step is suitably performed at 1,000° C. to 400° C., more preferably 1,000° C. to 600° C.
  • the purification step becomes more effective as its temperature increases.
  • the temperature exceeds 1,200° C.
  • shrinkage of a molded body proceeds to make it difficult for a gas to penetrate the inside of the molded body in the treatment with an atmosphere containing oxygen and/or water vapor in the next step, to thereby reduce the effect of repairing an oxygen-deficient defect. Therefore, the purification step is suitably performed at 1,200° C. to 800° C., more preferably 1,200° C. to 1,000° C.
  • the step of promoting repairing of an oxygen-deficient defect is suitably performed at 1,150° C. to 800° C., more preferably 1,100° C. to 950° C.
  • the silica powder serving as a main raw material or any of various additives contains a metallic element as an impurity, crystallization is accelerated in various heat treatments, and in particular, as a heat treatment temperature increases, the rate of the crystallization increases.
  • the Al concentration of the silica powder is preferably 70 ppm or less.
  • the glass member When the molding step is performed with a metal mold, the glass member can be produced in a larger quantity and more inexpensively than by prior art grinding and polishing processing, and hence a great contribution can be made to the widespread use of ultraviolet LEDs.
  • Injection molding, press molding, transfer molding, or the like may be suitably used as a molding method.
  • the silica glass member for hermetic sealing of the present invention can be suitably manufactured.
  • plastic matter refers to a kneaded product of silica glass powder, in a state of having higher viscosity than a slurry, and having hardness and plasticity comparable to those of a clay.
  • the formed plastic matter is degassed by being further kneaded under reduced pressure.
  • kneading extrusion is performed using a kneading extrusion molding machine manufactured by Miyazaki Iron Works Co., Ltd. under a reduced pressure of 0.1 MPa, with the result that the generation of bubbles after sintering can be reduced to a required degree.
  • the plastic matter subjected to the degassing treatment was injection-molded into a metal mold at an increased pressure of 120 MPa to provide a molded body having a predetermined shape.
  • the surface roughness of a sealing portion of a plain surface portion needs to be finished to 0.1 ⁇ m or less, preferably 0.05 ⁇ m or less in terms of Ra value.
  • the surface roughness of a lens-like projecting portion also needs to be finished to 0.1 ⁇ m or less, preferably 0.05 ⁇ m or less in terms of Ra value.
  • a plain surface part for sealing needs to satisfy very high flatness in order to realize hermetic sealing, but in the case of a metal mold, sufficient flatness can be realized even with general processing accuracy.
  • the removed molded body (hereinafter green body) was air-dried in a clean atmosphere having a cleanliness level of about 10,000 at room temperature for about 12 hours.
  • the green body after the drying was put in a silica glass container having a flat bottom portion, and together with the container, was subjected to heat treatment in a horizontal tubular furnace having a furnace core tube made of silica glass under various atmospheres and temperatures.
  • the temperature in the furnace was increased from room temperature at a temperature increase rate of 20° C./min to 800° C. and kept thereat.
  • the atmosphere at the time of the temperature increase is 100% nitrogen.
  • nitrogen was stopped, and the temperature was kept for 1 hour while oxygen was flowed at a concentration of 100%.
  • organic matter, such as METOLOSE contained in the green body was completely oxidized and removed.
  • the oxygen was switched to 100% nitrogen, and the temperature in the furnace was again increased at a temperature increase rate of 20° C./min to 1,200° C. and kept thereat.
  • the nitrogen was switched to 100% hydrogen chloride, and purification treatment with hydrogen chloride was performed for 1 hour.
  • the purification treatment reduces the concentrations of metal impurities, such as an alkali metal, iron, and copper, in silica glass.
  • hydrogen chloride gas reacts with Si—OH in the silica glass to form a Si—Cl bond, and hence, when the green body after the purification treatment is sintered as it is, the following reaction occurs: 2Si.Cl ⁇ Si ⁇ Si+Cl 2 .
  • the Si ⁇ Si bond is a structural defect called an oxygen-deficient defect.
  • the Si ⁇ Si bond has absorption at a wavelength of 245 nm, and at the same time, has extremely weak resistance to ultraviolet light. Accordingly, the defect is not suited for the purpose of the present invention, and hence needs to be cured.
  • the hydrogen chloride serving as the atmosphere gas was switched to 100% nitrogen, and the furnace temperature was decreased at a temperature decrease rate of 20° C./min to 1,050° C. and kept at 1,050° C.
  • the nitrogen was switched to 100% oxygen, and the temperature was kept for 1 hour.
  • the oxygen was replaced with nitrogen, followed by cooling to room temperature, and the resultant was removed.
  • the removed green bodies were arranged on a smooth carbon plate with their convex portions facing up, and were placed in a vacuum furnace.
  • the inside of a vacuum chamber was evacuated to a vacuum (1 ⁇ 10 ⁇ 2 Pa), and then the temperature was increased at a temperature increase rate of 20° C./min to 1,650° C., and kept at 1,650° C. for 20 minutes while a vacuum break (normal pressure 10 MPa) was performed with nitrogen. After that, electricity was turned off to cool the furnace. After 10 hours, the resultant was removed.
  • a silica glass member for LED hermetic sealing of interest was obtained.
  • the surface roughness of a sealing portion (substrate joining plain surface) and a convex portion were measured with a Mitutoyo surface roughness meter. The results are shown in Table 1. It was confirmed that the surface roughness of each of the portions fell within a predetermined range. In Table 1, measurement results at three measurement points (n) are shown.
  • Transmittance measurement cannot be performed for a lens shape. Therefore, a transparent flat plate measuring 20 mm ⁇ 20 mm ⁇ 2 mm was produced using exactly the same materials and manufacturing method as those of Example 1 and subjected to general transmittance measurement (measurement apparatus: UV/VIS/NIR SPECTROMETER LAMBDA 900 manufactured by PerkinElmer, Inc.). The results are shown in Table 2 and FIG. 6 (graphical representation of an apparent transmittance and a theoretical transmittance). An internal transmittance for ultraviolet light having a wavelength of 300 nm to 400 nm and an internal transmittance for ultraviolet light having a wavelength of 245 nm or more and less than 300 nm were determined from the apparent transmittance by the calculation expression shown below. The internal transmittances are shown in Table 2. It was confirmed that each of the internal transmittances fell within a predetermined range.
  • Transmittance Measurement with Integrating Sphere measured using measurement apparatus: UV/VIS/NIR SPECTROMETER LAMBDA 900 manufactured by PerkinElmer, Inc., integrating sphere: MODEL#150MM RSA ASSY.
  • Table 3 The results are shown in Table 3 and FIG. 7 together with the results of the general transmittance measurement, and calculated differences therebetween are shown in Table 3. As apparent from Table 3, it was confirmed that the differences each fell within a predetermined range.
  • the maximum value of a bubble class was taken as a diameter (for example, calculation was performed assuming 20 ⁇ m to 30 ⁇ m as a diameter of 30 ⁇ m). It was confirmed that the use of silica glass having such cross-sectional area of bubbles enabled use as a silica glass member for hermetic sealing for an SMD package with a sufficiently suppressed scattering intensity.
  • OH Group Concentration The OH group concentration of a silica glass sample measuring 20 mm ⁇ 20 mm ⁇ 2 mm produced using the same materials and manufacturing method as those of Example 1 was measured with an infrared spectrophotometer, and as a result, the contained OH group concentration was found to be 1.3 ppm. Further, in the oxygen treatment of Example 1, the oxygen was humidified by bubbling with water, and as a result, a silica glass body having OH group concentration of 4.6 ppm was obtained. When each of those samples was irradiated with ultraviolet light having a wavelength of 254 nm, fluorescence was not observed. Thus, the samples were each found to be suited as a silica glass member for hermetic sealing for an SMD package for a UV-LED.
  • a planar silica glass plate material and a hemispherical lens were each independently produced, polished, and bonded to each other using any of adhesives A to E described below to produce a silica glass member having a shape similar to that of Example 1, which was subjected to transmittance measurement.
  • the results are shown in FIG. 8 .
  • the transmittance of the silica glass member of Example 1 is also shown.
  • all the silica glass members joined with the adhesives were found not to have sufficient transmission properties for UVB (falling within a wavelength range of from 315 nm to 280 nm) and UVC (falling within a wavelength range of from 280 nm to 200 nm).
  • the adhesives A to E are as described below.
  • Adhesive A vinyl chloride resin-based adhesive AR-066 manufactured by Cemedine Co., Ltd. (for bonding a vinyl chloride tube)
  • Adhesive B thermosetting silicone-based adhesive KE-1886 manufactured by Shin-Etsu Chemical Co., Ltd. (e.g., a rubber for electrical and electronic sealing)
  • Adhesive C water glass-based adhesive 37271-01 manufactured by Kanto Chemical Co., Inc. (for bonding ceramic or glass)
  • Adhesive D synthetic rubber-based adhesive #14331 manufactured by Konishi Co., Ltd. (for bonding leather, synthetic rubber, or urethane foam)
  • Adhesive E acrylic modified adhesive AX-033 manufactured by Cemedine Co., Ltd. (for bonding a metal, glass, or rubber)
  • the mixture of the silica powder and the binder subjected to the degassing treatment was injection-molded into a metal mold at an increased pressure of 120 MPa to provide a molded body having a predetermined shape.
  • an in-plane surface roughness needs to be finished to 0.1 ⁇ m or less, preferably 0.05 ⁇ m or less in terms of Ra value.
  • the thus produced molded body was air-dried in a clean atmosphere having a cleanliness level of about 10,000 at room temperature for about 12 hours.
  • the molded body after the drying was put in a quartz glass container having a flat bottom portion, and together with the container, was subjected to heat treatment in a horizontal tubular furnace having a furnace core tube made of quartz glass under various atmospheres and temperatures.
  • the following steps (a) to (c) were performed.
  • the temperature in the furnace was increased from room temperature at a temperature increase rate of 20° C./min to 800° C. and kept thereat.
  • the atmosphere at the time of the temperature increase is 100% nitrogen.
  • nitrogen was stopped, and the temperature was kept for 1 hour while oxygen was flowed at a concentration of 100%.
  • organic matter, such as METOLOSE contained in the molded body was completely oxidized and removed.
  • the oxygen was switched to 100% nitrogen, and the temperature in the furnace was again increased at a temperature increase rate of 20° C./min to 1,200° C. and kept thereat.
  • the nitrogen was switched to 100% hydrogen chloride, and purification treatment with hydrogen chloride was performed for 1 hour.
  • the purification treatment reduces the concentrations of metal impurities, such as an alkali metal, copper, and iron, in quartz glass. Meanwhile, hydrogen chloride reacts with Si—OH in the quartz glass to form a Si—Cl bond, and hence, when the molded body after the purification treatment is vitrified as it is, the following reaction occurs: 2Si ⁇ Cl ⁇ Si ⁇ Si+Cl 2 .
  • the Si ⁇ Si bond is a structural defect called an oxygen-deficient defect.
  • the Si ⁇ Si bond has absorption at a wavelength of about 250 nm, and at the same time, has extremely weak resistance to ultraviolet light. Accordingly, the defect is not suited for the purpose of the present invention, and hence needs to be cured.
  • the hydrogen chloride serving as the atmosphere gas was switched to 100% nitrogen, and the temperature was decreased at a temperature decrease rate of 20° C./min to 1,050° C. and kept thereat.
  • the nitrogen was switched to oxygen 100%, and treatment for repairing an oxygen-deficient defect in quartz glass with oxygen was performed for 1 hour. After the treatment, the oxygen was switched to 100% nitrogen, followed by cooling to room temperature, and the resultant was removed.
  • the removed molded bodies were arranged on a smooth carbon plate, and placed in a vacuum furnace.
  • the inside of a vacuum chamber was evacuated to a degree of vacuum of 1 ⁇ 10 ⁇ 2 Pa, and then the temperature was increased at a temperature increase rate of 20° C./min to 1,650° C. After having reached 1,650° C., the temperature was kept for 10 minutes while a vacuum break was performed with nitrogen to increase the pressure to 0.1 MPa. After that, electricity was turned off to cool the furnace. After 10 hours, the resultant was removed.
  • a quartz glass member for an ultraviolet LED of interest was obtained.
  • the obtained quartz glass member was decomposed with hydrofluoric acid, and subjected to measurement by ICP emission spectrometry.
  • the obtained quartz glass member was visually observed.
  • a case of transparent quartz glass was evaluated as “Satisfactory”
  • a case of being opaque due to crystallization (devitrification) was evaluated as “Crystallization”
  • a case of containing visually recognizable bubbles was evaluated as “Bubbles”.
  • a flat plate measuring 20 mm ⁇ 20 mm ⁇ 2 mm was produced, and subjected to measurement with a UV-VIS spectrophotometer in the wavelength range of from 200 nm to 400 nm to confirm the presence or absence of absorption at a wavelength of 250 nm.
  • a case in which absorption at a wavelength of 250 nm was absent was evaluated as “Absent”, a case in which the absorption was present was evaluated as “Present”, and a case in which crystallization made measurement impossible was evaluated as “Unmeasurable”.
  • Table 5 The transmittance measurement results of the quartz glass member for an ultraviolet LED obtained in Example 2 at wavelengths of from 200 nm to 400 nm are shown in FIG. 9 .
  • a quartz glass member for an ultraviolet LED was obtained in the same manner as in Example 2 except that the treatment for repairing an oxygen-deficient defect was performed at a temperature of 1,050° C., and under an atmosphere containing water vapor produced by a method involving bubbling pure water kept at 30° C. with oxygen serving as a carrier.
  • the quartz glass member for an ultraviolet LED obtained in Example 2 was subjected to hydrogen treatment in a hydrogen atmosphere at 400° C. and 0.8 MP (heating treatment with a hydrogen atmosphere) to introduce hydrogen molecules into the glass.
  • a quartz glass member for an ultraviolet LED was obtained.
  • a quartz glass member for an ultraviolet LED was obtained by performing the same treatments as in Example 2 except that mixed powder obtained by mixing powder having an average particle diameter of 0.25 ⁇ m (ADMAFINE SO-E1 manufactured by Admatechs Company Limited), powder having an average particle diameter of 1.0 ⁇ m (ADMAFINE SO-E3 manufactured by Admatechs Company Limited), and powder having an average particle diameter of 2.0 ⁇ m (ADMAFINE SO-E5 manufactured by Admatechs Company Limited) at a weight ratio of 1:1:2 was used as a raw material.
  • a quartz glass member was obtained in the same manner as in Example 2 except that the step of promoting repairing of an oxygen-deficient defect was not performed.
  • the transmittance measurement results of the quartz glass member obtained in Comparative Example 2 at wavelengths of from 200 nm to 400 nm are shown in FIG. 10 .
  • Treatments were performed in the same manner as in Example 2 except that the degreasing temperature of the degreasing step in the heat treatment step was set to 1,100° C.
  • the state after the heat treatment step was not particularly different from that of the sample of Example 2, and hence the sample of Comparative Example 3 was subjected to vitrification, but became opaque due to crystallization.
  • Treatments were performed in the same manner as in Example 2 except that the purification temperature of the purification step in the heat treatment step was set to 1,350° C. Although the volume of the sintered body after the heat treatment step was slightly shrunk, the sintered body was subjected to vitrification as it was. As a result, a large number of extremely fine bubbles were mixed therein.
  • Treatments were performed in the same manner as in Example 2 except that the oxygen defect repairing temperature of the step of promoting repairing of an oxygen-deficient defect in the heat treatment step was set to 1,200° C.
  • the state after the heat treatment was not particularly different from that of the sample of Example 2, and hence the sample of Comparative Example 5 was subjected to vitrification, but became opaque due to crystallization.
  • the glass member obtained in Comparative Example 2 was kept in an oxygen atmosphere at 1,100° C. for 10 hours.
  • the transmittance of the resultant sample was measured. As a result, it was found that, although absorption at a wavelength of 250 nm was slightly improved, the transmittance in the entire region of from 200 nm to 400 nm was reduced due to the influence of contamination caused by the heat treatment.
  • 10 silica glass member for hermetic sealing
  • 10 A silica glass substrate
  • 14 hermetic sealing container
  • 16 bottom wall
  • 18 side wall
  • 20 opening
  • 22 upper end outer peripheral portion
  • 22 a container outer periphery joining plain surface
  • 24 first surface
  • 24 a substrate joining plain surface
  • 26 second surface
  • 28 lens-like convex portion
  • 30 connecting flat portion
  • 32 hollow portion
  • 34 hanging enlarged portion.

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US20220115570A1 (en) 2022-04-14
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