EP1373151A1 - Dopage a l'oxygene de verre d'oxyfluorure de silicium - Google Patents

Dopage a l'oxygene de verre d'oxyfluorure de silicium

Info

Publication number
EP1373151A1
EP1373151A1 EP02714956A EP02714956A EP1373151A1 EP 1373151 A1 EP1373151 A1 EP 1373151A1 EP 02714956 A EP02714956 A EP 02714956A EP 02714956 A EP02714956 A EP 02714956A EP 1373151 A1 EP1373151 A1 EP 1373151A1
Authority
EP
European Patent Office
Prior art keywords
silicon oxyfluoride
oxyfluoride glass
glass
absoφtion
atmosphere
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Withdrawn
Application number
EP02714956A
Other languages
German (de)
English (en)
Inventor
Lisa A. MOORE
Charlene M. SMITH
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.)
Corning Inc
Original Assignee
Corning Inc
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Priority claimed from US09/997,782 external-priority patent/US6502426B2/en
Application filed by Corning Inc filed Critical Corning Inc
Publication of EP1373151A1 publication Critical patent/EP1373151A1/fr
Withdrawn legal-status Critical Current

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Classifications

    • 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
    • G—PHYSICS
    • G03—PHOTOGRAPHY; CINEMATOGRAPHY; ANALOGOUS TECHNIQUES USING WAVES OTHER THAN OPTICAL WAVES; ELECTROGRAPHY; HOLOGRAPHY
    • G03F—PHOTOMECHANICAL PRODUCTION OF TEXTURED OR PATTERNED SURFACES, e.g. FOR PRINTING, FOR PROCESSING OF SEMICONDUCTOR DEVICES; MATERIALS THEREFOR; ORIGINALS THEREFOR; APPARATUS SPECIALLY ADAPTED THEREFOR
    • G03F7/00—Photomechanical, e.g. photolithographic, production of textured or patterned surfaces, e.g. printing surfaces; Materials therefor, e.g. comprising photoresists; Apparatus specially adapted therefor
    • G03F7/70—Microphotolithographic exposure; Apparatus therefor
    • G03F7/70216—Mask projection systems
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
    • C03B19/00—Other methods of shaping glass
    • C03B19/14—Other methods of shaping glass by gas- or vapour- phase reaction processes
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
    • C03B19/00—Other methods of shaping glass
    • C03B19/14—Other methods of shaping glass by gas- or vapour- phase reaction processes
    • C03B19/1407—Deposition reactors therefor
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
    • C03B19/00—Other methods of shaping glass
    • C03B19/14—Other methods of shaping glass by gas- or vapour- phase reaction processes
    • C03B19/1415—Reactant delivery systems
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
    • C03B19/00—Other methods of shaping glass
    • C03B19/14—Other methods of shaping glass by gas- or vapour- phase reaction processes
    • C03B19/1415—Reactant delivery systems
    • C03B19/1423—Reactant deposition burners
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
    • C03B19/00—Other methods of shaping glass
    • C03B19/14—Other methods of shaping glass by gas- or vapour- phase reaction processes
    • C03B19/1453—Thermal after-treatment of the shaped article, e.g. dehydrating, consolidating, sintering
    • 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
    • G03—PHOTOGRAPHY; CINEMATOGRAPHY; ANALOGOUS TECHNIQUES USING WAVES OTHER THAN OPTICAL WAVES; ELECTROGRAPHY; HOLOGRAPHY
    • G03F—PHOTOMECHANICAL PRODUCTION OF TEXTURED OR PATTERNED SURFACES, e.g. FOR PRINTING, FOR PROCESSING OF SEMICONDUCTOR DEVICES; MATERIALS THEREFOR; ORIGINALS THEREFOR; APPARATUS SPECIALLY ADAPTED THEREFOR
    • G03F1/00—Originals for photomechanical production of textured or patterned surfaces, e.g., masks, photo-masks, reticles; Mask blanks or pellicles therefor; Containers specially adapted therefor; Preparation thereof
    • G03F1/60—Substrates
    • G—PHYSICS
    • G03—PHOTOGRAPHY; CINEMATOGRAPHY; ANALOGOUS TECHNIQUES USING WAVES OTHER THAN OPTICAL WAVES; ELECTROGRAPHY; HOLOGRAPHY
    • G03F—PHOTOMECHANICAL PRODUCTION OF TEXTURED OR PATTERNED SURFACES, e.g. FOR PRINTING, FOR PROCESSING OF SEMICONDUCTOR DEVICES; MATERIALS THEREFOR; ORIGINALS THEREFOR; APPARATUS SPECIALLY ADAPTED THEREFOR
    • G03F7/00—Photomechanical, e.g. photolithographic, production of textured or patterned surfaces, e.g. printing surfaces; Materials therefor, e.g. comprising photoresists; Apparatus specially adapted therefor
    • G03F7/70—Microphotolithographic exposure; Apparatus therefor
    • G03F7/708—Construction of apparatus, e.g. environment aspects, hygiene aspects or materials
    • G03F7/7095—Materials, e.g. materials for housing, stage or other support having particular properties, e.g. weight, strength, conductivity, thermal expansion coefficient
    • G03F7/70958—Optical materials or coatings, e.g. with particular transmittance, reflectance or anti-reflection properties
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
    • C03B2201/00—Type of glass produced
    • C03B2201/06—Doped silica-based glasses
    • C03B2201/07—Impurity concentration specified
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
    • C03B2201/00—Type of glass produced
    • C03B2201/06—Doped silica-based glasses
    • C03B2201/07—Impurity concentration specified
    • C03B2201/075—Hydroxyl ion (OH)
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
    • C03B2201/00—Type of glass produced
    • C03B2201/06—Doped silica-based glasses
    • C03B2201/08—Doped silica-based glasses doped with boron or fluorine or other refractive index decreasing dopant
    • C03B2201/12—Doped silica-based glasses doped with boron or fluorine or other refractive index decreasing dopant doped with fluorine
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
    • C03B2201/00—Type of glass produced
    • C03B2201/06—Doped silica-based glasses
    • C03B2201/20—Doped silica-based glasses doped with non-metals other than boron or fluorine
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
    • C03B2201/00—Type of glass produced
    • C03B2201/06—Doped silica-based glasses
    • C03B2201/20—Doped silica-based glasses doped with non-metals other than boron or fluorine
    • C03B2201/21—Doped silica-based glasses doped with non-metals other than boron or fluorine doped with molecular hydrogen
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
    • C03B2207/00—Glass deposition burners
    • C03B2207/30—For glass precursor of non-standard type, e.g. solid SiH3F
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
    • C03B2207/00—Glass deposition burners
    • C03B2207/30—For glass precursor of non-standard type, e.g. solid SiH3F
    • C03B2207/32—Non-halide
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
    • C03B2207/00—Glass deposition burners
    • C03B2207/36—Fuel or oxidant details, e.g. flow rate, flow rate ratio, fuel additives
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
    • C03B2207/00—Glass deposition burners
    • C03B2207/36—Fuel or oxidant details, e.g. flow rate, flow rate ratio, fuel additives
    • C03B2207/38—Fuel combinations or non-standard fuels, e.g. H2+CH4, ethane
    • 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
    • C03C2201/08—Doped silica-based glasses containing boron or halide
    • C03C2201/12—Doped silica-based glasses containing boron or halide containing fluorine
    • 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
    • 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
    • C03C2201/21—Doped silica-based glasses containing non-metals other than boron or halide containing molecular hydrogen
    • 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
    • C03C2201/06—Doped silica-based glasses
    • C03C2201/30—Doped silica-based glasses containing metals
    • 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
    • C03C2201/30—Doped silica-based glasses containing metals
    • C03C2201/32—Doped silica-based glasses containing metals containing aluminium
    • 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

Definitions

  • the present invention relates generally to lithography, and particularly to optical photolithography glass for use in optical photolithography systems utilizing vacuum ultraviolet light (NUN) wavelengths below 193 nm, preferably below 175nm, preferably below 164 nm, such as VUV projection lithography systems utilizing wavelengths in the 157 nm region.
  • NUN vacuum ultraviolet light
  • the invention relates to VUV transmitting glass that is transmissive at wavelengths below 193 nm, in particular, a photomask silicon oxyfluoride glass suitable for use in the Vacuum Ultraviolet (VUV) 157 nm wavelength region.
  • VUV Vacuum Ultraviolet
  • Refractive optics requires materials having high transmittance.
  • high purity fused silica has been shown to exhibit the required transmittance of 99%/cm or better.
  • Projection optical photolithography systems that utilize the vacuum ultraviolet wavelengths of light below 193 nm provide benefits in terms of achieving smaller feature dimensions. Such systems that utilize vacuum ultraviolet wavelengths in the 157 nm wavelength region have the potential of improving integrated circuits with smaller feature sizes.
  • Current optical lithography systems used by the semiconductor industry in the manufacture of integrated circuits have progressed towards shorter wavelengths of light, such as the popular 248 nm and 193 nm wavelengths, but the commercial use and adoption of vacuum ultraviolet wavelengths below 193nm, such as 157 nm has been hindered by the transmission nature of such vacuum ultraviolet wavelengths in the 157 nm region through optical materials.
  • the glass preferably has ⁇ 1% transmission loss at 157.6nm after exposure to the F 2 excimer laser for 60 million at 0.1mJ/cm 2 -pulse.
  • Our invention describes silicon oxyfluoride glasses containing high levels of molecular oxygen that exhibit lower F 2 laser-induced absorption compared to non-oxygen loaded glasses and methods for making them.
  • the invention includes a method of making a VUV transmitting glass for transmitting below 200 nm VUV wavelengths such as 157 nm wavelengths produced by F 2 excimer lasers.
  • the method includes providing a silicon oxyfluoride glass, providing a plurality of O 2 molecules, and doping the O 2 molecules into the silicon oxyfluoride glass to provide a VUV transmitting silicon oxyfluoride glass containing intersticial O 2 molecules.
  • the invention includes a method of making a laser durable VUV transmitting silicon oxyfluoride glass, which is preferably durable to F 2 excimer laser exposure with a resistance to F 2 laser induced absorption.
  • the method includes providing a consolidated silicon oxyfluoride glass and providing an O 2 doping treatment atmosphere.
  • the method includes enveloping the silicon oxyfluoride glass with the O 2 doping treatment atmosphere and dissolving a plurality of the O 2 molecules from the atmosphere into the silicon oxyfluoride glass to provide a silicon oxyfluoride glass with insolution O 2 molecules.
  • the invention includes a method of making a laser durable VUV transmitting silicon oxyfluoride glass.
  • the method includes providing a non-consolidated silicon oxyfluoride glass precursor and providing a glass consolidation furnace with a heated consolidation zone for consolidating the non-consolidated glass precursor.
  • the method includes supplying an oxygen doping atmosphere to the consolidation furnace and consolidating the glass precursor into a consolidated silicon oxyfluoride glass wherein O 2 molecules are dissolved in the consolidated silicon oxyfluoride glass.
  • the invention includes a VUV transmitting glass photomask substrate.
  • the photomask substrate is comprised of a silicon oxyfluoride glass doped with a plurality of O 2 molecules.
  • the invention includes a VUV transmitting silicon oxyfluoride glass.
  • the VUV transmitting silicon oxyfluoride glass contains a plurality of doped O 2 molecules and has a resistance to VUV laser induced absorption bands.
  • FIG. 1 shows a method and glass in accordance with the invention.
  • FIG. 2 shows a method and glass in accordance with the invention.
  • FIG. 3 shows a method, a VUV lithography system, and glass in accordance with the invention.
  • FIG. 4 shows a method, a VUV lithography system, and glass in accordance with the invention.
  • FIG. 5 shows a VUV transmitting silicon oxyfluoride glass photomask substrate in accordance with the invention (FIG. 5A top view, FIG. 5B side view).
  • FIG. 6 shows a VUV absorption spectra of a silicon oxyfluoride glass before exposure to a F 2 excimer laser (open circles), after exposing to the F 2 excimer laser for 10.6E6 pulses at 2 mj/cm 2 -pulse (open squares), and after F 2 excimer laser exposure and oxygen treatment (1 atmosphere O 2 for 7 days at 1000 degrees C)(closed diamonds).
  • FIG. 7 shows a VUV absorption spectra of silicon oxyfluoride glass that was heat treated in oxygen (open circles), then exposed to the F2 excimer laser for 9.92E6 pulses at 2 mJ/cm 2 -pulse (closed diamonds).
  • a VUV absorption spectra curve for the same glass without an oxygen pretreatment exposed to the same laser conditions (10.6E6 pulses at 2 mJ/cm 2 -pulse, open squares) is included for comparison.
  • the invention includes a method of making a VUV transmitting glass.
  • the VUV transmitting glass provides for transmission of below 200 nm VUV wavelengths, such as the 157 nm wavelength emissions of a F 2 excimer laser.
  • the VUV transmitting glass is durable to F 2 excimer laser exposures and has a resistance to F 2 laser induced absorption.
  • the method includes the steps of providing a silicon oxyfluoride glass and providing a plurality of O 2 molecules.
  • the method includes doping the O 2 molecules into the silicon oxyfluoride glass to provide a VUV transmitting silicon oxyfluoride glass containing intersticial O 2 molecules.
  • Providing a silicon oxyfluoride glass preferably includes providing a silicon oxyfluoride glass which contains > 0.1 wt.
  • Providing a silicon oxyfluoride glass preferably includes providing a dry silicon oxyfluoride glass which has an OH content below 50 ppm by weight.
  • the dry silicon oxyfluoride glass has ⁇ 10 ppm OH by weight, more preferably ⁇ 5 ppm OH by weight, and most preferably ⁇ 1 ppm OH by weight.
  • Providing a silicon oxyfluoride glass preferably includes providing a silicon oxyfluoride glass which has a CI content below 5 ppm by weight, more preferably ⁇ 1 ppm CI by weight.
  • Doping the O 2 molecules preferably includes dissolving the O 2 molecules into the silicon oxyfluoride glass, preferably with the method including causing the O 2 molecules to pass into solution in the glass and remain as O 2 molecules in the glass when the method of making is completed and the glass is put into use for transmitting light wavelengths.
  • the O 2 molecules remain as O 2 molecules in the glass at the end of the making process, with the glass containing such intersticial O 2 molecules as insolution O 2 molecules.
  • FIG. 1 shows an embodiment of the method of making the VUV transmitting glass 20.
  • the method includes providing an O 2 doping treatment atmosphere 26 which has an O 2 concentration of at least 10 15 O 2 mole/cc.
  • the O 2 doping treatment atmosphere has a concentration of > 10 16 O 2 moles/cc.
  • the O 2 doping treatment atmosphere has a concentration of ⁇ 10 20 O 2 moles/cc.
  • a particularly preferred range of O 2 concentration is in the range of about 10 16 to 10 20 O 2 moles/cc.
  • the method preferably includes providing an O 2 doping vessel 28 for containing the O 2 doping treatment atmosphere and silicon oxyfluoride glass 22.
  • the method preferably includes heating treatment atmosphere 26 and glass 22 to a predetermined O 2 doping temperature which is effective for doping the molecules of O 2 into the glass.
  • the O2 doping temperature is at least 600° C.
  • the O 2 doping treatment atmosphere is at least one atmosphere of O 2 .
  • the invention includes hipping the glass 22 so that the glass is hot isostatically pressed in the presence of that O 2 molecules.
  • the invention includes pressurizing the interior of the O 2 doping vessel so that the glass 22 is doped with O 2 from a pressurized O 2 treatment atmosphere.
  • the 0 2 doping treatment vessel 28 is comprised of a non-contaminant refractory material. More preferably the non-contaminating refractory material treatment vessel is non-metallic such as a silica quartz muffle furnace or a non-metallic bell jar. As shown in FIG.
  • the method includes consolidating the silicon oxyfluoride glass in the presence of, and with, the O 2 molecules.
  • the non-consolidated glass 24 is consolidated into consolidated glass 22 in the presence of the O 2 molecules so that the resulting consolidated silicon oxyfluoride glass 20 contains doped O 2 molecules.
  • the invention includes a method of making a laser durable VUV transmitting silicon oxyfluoride glass.
  • the method includes providing a consolidated silicon oxyfluoride glass 22.
  • the method includes providing a O 2 doping treatment atmosphere.
  • the method includes enveloping the silicon oxyfluoride glass with the O2 doping treatment atmosphere and dissolving a plurality of the O 2 molecules from the atmosphere into the silicon oxyfluoride glass to provide a silicon oxyfluoride glass with insolution O 2 molecules.
  • vessel 28 contains consolidated glass 22 and O 2 molecule atmosphere 26 provided by the O 2 supply source so that the glass is enveloped in the O 2 doping treatment atmosphere.
  • the method includes heating the O 2 doping treatment atmosphere and the silicon oxyfluoride glass to a predetermined O 2 doping temperature, preferably at > 600° C.
  • a preferred O 2 doping temperature is about 1000 ( ⁇ 100) degrees C, most preferably with about one atmosphere of oxygen.
  • Providing an O2 doping treatment atmosphere 26 preferably includes providing an atmosphere with an O concentration of at least 10 15 O 2 moles/cc, more preferably at least 10 16 O 2 moles/cc.
  • the atmosphere O 2 concentration is no greater than 10 O 2 moles/cc.
  • a preferred O 2 concentration doping treatment atmosphere range is about 10 16 - 10 18 O 2 moles/cc.
  • the invention includes a method of making a laser durable VUV transmitting silicon oxyfluoride glass.
  • An embodiment of the invention is shown in FIG. 2.
  • the method includes providing a non-consolidated silicon oxyfluoride glass precursor 24.
  • the method includes providing a glass consolidation furnace 30 with a heated consolidation zone 32 for consolidating the non-consolidated glass precursor.
  • the method includes supplying an oxygen doping atmosphere 26 to the consolidating furnace 30 and consolidating the glass precursor into a consolidated silicon oxyfluoride glass wherein O 2 molecules are dissolved in the consolidated silicon oxyfluoride glass.
  • the ' method includes heating the oxygen doping atmosphere and the consolidating glass 24 to a predetermined O 2 doping consolidation temperature.
  • providing a glass consolidation furnace 30 includes providing a non- contaminant refractory material non-metallic silica muffle furnace.
  • providing a glass consolidation furnace 30 includes providing a plasma discharge glass consolidation furnace.
  • the plasma discharge of the plasma discharge glass consolidating furnace is utilized to heat and consolidate the non-consolidate precursor into the consolidated glass in the presence of the O 2 .
  • non- consolidated glass particles or other Si containing feedstocks are fed into a plasma discharge along with oxygen in a direct laydown plasma process.
  • Supplying an oxygen doping atmosphere preferably includes supplying an atmosphere with an O 2 concentration of at least 10 15 O 2 moles/cc, more preferably > 10 16 O2 moles/cc.
  • the oxygen doping atmosphere has an O 2 concentration no greater than 10 O 2 moles/cc.
  • the doping atmosphere has an O 2 concentration in the range of 10 16 to 10 18 moles/cc.
  • the non-consolidated glass is a soot body preform, the glass is consolidated under a highly oxidizing atmosphere which is at least 50% by volume O 2 .
  • the O 2 doped glass is thus consolidated and synthesized so as to contain O 2 molecules.
  • the invention includes a VUV transmitting glass photomask substrate.
  • FIGs. 3- 5 show a VUV transmitting glass photomask substrate 34.
  • the VUV transmitting glass photomask substrate 34 is comprised of a silicon oxyfluoride glass doped with a plurality of O 2 molecules.
  • the silicon oxyfluoride glass contains at least 0.1 weight percent fluorine, more preferably a fluorine content in the range of 0.1 to 2 wt. % F.
  • a preferred fluorine content range is from 0.2 to 1.2 wt. % F.
  • a preferred fluorine content range is from 0.1 to 0.4 wt. % F.
  • a preferred fluorine content is about 1.2 ( ⁇ 0.3) wt. % F.
  • the silicon oxyfluoride glass doped with O 2 is a dry glass, preferably with an OH content below 50 ppm by weight.
  • the O 2 doped low OH silicon oxyfluoride glass photomask substrate blank 34 has an OH content ⁇ 10 ppm by wt., more preferred ⁇ 5 ppm by wt., and most preferred ⁇ 1 ppm by wt.
  • the dry silicon oxyfluoride glass doped with O 2 has a CI content below 5 ppm by weight, and more preferred ⁇ 1 ppm CI by weight.
  • the photomask substrate glass has a 165 nm absorption less than 0.2 absorption units/5.1 mm.
  • the photomask substrate glass has a 215 nm absorption less than 0.2 absorption units/5.1 mm.
  • the silicon oxyfluoride glass has a resistance to F2 excimer 157 nm laser induced 165 nm absorption bands.
  • the silicon oxyfluoride glass has a 165 nm absorption less than 0.3 absorption units/5.1 mm after an F 2 excimer laser exposure of at least 9.92 E6 pulses at 2mJ/cm -pulse.
  • the silicon oxyfluoride glass has a 215 nm absorption less than 0.2 absorption units/5.1 mm after an F 2 excimer laser exposure of at least 9.92 E6 pulses at 2mJ/cm -pulse.
  • the silicon oxyfluoride glass has a laser induced absorption at 157 nm less than 0.4 absorption units/5 mm after an F 2 excimer laser exposure of at least 9.92 E6 pulses at 2mJ/cm 2 -pulse.
  • the silicon oxyfluoride glass substrate has a 157 nm laser induced delta absorption ⁇ 0.20 absorption units/5 mm after an F 2 excimer laser exposure of at least 9.92 E6 pulses at 2mJ/cm -pulse.
  • the invention includes a VUV transmitting silicon oxyfluoride lithography glass for transmitting wavelengths below 200 nm.
  • the VUV transmitting silicon oxyfluoride glass of the invention is shown by the cross hatching in FIGs. 3-4.
  • the inventive VUV transmitting silicon oxyfluoride glass contains a plurality of doped O 2 molecules and has a resistance to VUV laser induced absorption bands.
  • the VUV transmitting glass is comprised of a silicon oxyfluoride glass doped with a plurality of intersticial O 2 molecules.
  • the silicon oxyfluoride glass contains at least 0.1 weight percent fluorine, more preferably a fluorine content in the range of 0.1 to 2 wt. % F.
  • a preferred fluorine content range is from 0.2 to 1.2 wt. % F.
  • a preferred fluorine content range is from 0.1 to 0.4 wt. % F.
  • a preferred fluorine content is about 1.2 ( ⁇ 0.3) wt. % F.
  • the silicon oxyfluoride glass doped with O 2 is a dry glass, preferably with an OH content below 50 ppm by weight.
  • the O 2 doped low OH silicon oxyfluoride glass has an OH content ⁇ 10 ppm by wt., more preferred ⁇ 5 ppm by wt., and most preferred ⁇ 1 ppm by wt.
  • the dry silicon oxyfluoride glass doped with O 2 has a CI content below 5 ppm by weight, and more preferred ⁇ 1 ppm CI by weight.
  • the glass has a 165 nm absorption less than 0.2 absorption units/5.1 mm.
  • the glass has a 215 nm absorption less than 0.2 absorption units/5.1 mm.
  • the silicon oxyfluoride glass has a resistance to F 2 excimer 157 nm laser induced 165 nm absorption bands.
  • the silicon oxyfluoride glass has a 165 nm absorption less than 0.3 absorption units/5.1 mm after an F 2 excimer laser exposure of at least 9.92 E6 pulses at 2mJ/cm -pulse.
  • the silicon oxyfluoride glass has a 215 nm absorption less than 0.2 absorption units/5.1 mm after an F 2 excimer laser exposure of at least 9.92 E6 pulses at 2mJ/cm -pulse.
  • the silicon oxyfluoride glass has a laser induced absorption at 157 nm less than 0.4 absorption units/5 mm after an F 2 excimer laser exposure of at least 9.92 E6 pulses at 2mJ/cm 2 -pulse.
  • the silicon oxyfluoride glass has a 157 nm laser induced delta absorption ⁇ 0.20 absorption units/5 mm after an F 2 excimer laser exposure of at least 9.92 E6 pulses at 2mJ/cm -pulse.
  • FIG. 6 shows the VUV spectra of a dry ( ⁇ 1 ppm OH), silicon oxyfluoride-doped (1.2 wt.%F) glass as made (open circles, lowest curve) and then after being exposed to 10.6E6 pulses at 2 mJ/cm 2 -pulse at 157nm (open squares, highest curve). The appearance of the E' center at 215nm as well as the more important 165nm band (ODC) is clear. This glass was then held under oxygen (1 atm) at 1000°C for 7 days.
  • FIG. 7 shows the VUV spectra of the same silicon oxyfluoride glass as in FIG. 6 that was pre-treated in oxygen (open circles, lowest curve), then exposed to the F 2 excimer laser for 9.92E6 pulses at 2 mJ/cm 2 -pulse (closed diamonds, middle curve).
  • the open circles lowest curve spectrum is the glass after O 2 -loading, before exposure.
  • the closed diamonds middle curve spectrum is the O 2 -loaded glass exposed at 157nm for about 10E6 pulses, and the open squares highest curve spectrum is the same as in FIG. 6, of the glass as made, exposed to 10.6E6 pulses (for comparison).
  • the feature to notice in the comparison is the lack of a 165nm band (ODC) in the O 2 -containing glass.
  • ODC 165nm band
  • the presence of oxygen inhibits the formation of the 165nm band. Since the 165nm band is close to 157nm, reducing this absorption band significantly reduces the induced absorption at 157nm.
  • Silicon oxyfluoride glasses containing excess oxygen can be made by several methods. First, as described above, the as-made silicon oxyfluoride glasses glass can be exposed to an oxygen atmosphere at elevated temperatures to diffuse O 2 into the structure. Second, the glass can be synthesized so as to contain excess oxygen. Silica glasses made by direct laydown processes(e.g., plasma) have been made with high excess oxygen levels compared to glasses made by soot preform body-to-consolidated glass body processes. Finally, the oxygen content of silicon oxyfluoride glasses made by soot preform body -to- consolidated glass body processing can be increased by consolidating under a highly oxidizing atmosphere (e.g. 50-100% O 2 ). The invention provides silicon oxyfluoride glasses with improved resistance to
  • inventive silicon oxyfluoride glasses materials are useful for 157nm lithography applications such as photomasks, lenses, pellicles, and windows, for example.

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Abstract

L'invention concerne un verre d'oxyfluorure de silicium pur qui peut être utilisé comme substrat de masque photographique dans des applications de photolithographie dans la région des longueurs d'ondes UV extrême inférieures à 190nm. On produit ce verre (20) dopé en faisant entrer en contact une atmosphère (26) de dopage O2 avec un verre (22) d'oxyfluorure de silicium dans une enceinte (28) de dopage. Ce verre d'oxyfluorure de silicium est transmissif à des longueurs d'ondes de l'ordre de 157 nm, ce qui le rend particulièrement utile en tant que substrat de masque photographique dans la région de longueur d'onde de 157 nm. Le substrat de masque photographique décrit est un verre d'oxyfluorure de silicium « sec » qui contient des molécules O2 dopées et qui présente un facteur de transmission et une durabilité à transmission laser très élevés pour les longueurs d'onde de la région ultraviolet extrême (UV extrême). Outre du fluorure, et une quantité réduite voire nulle de OH, ce verre d'oxyfluorure de silicium contient des molécules d'O2 interstitielles qui lui confèrent une résistance accrue à l'insolation par laser. Ce verre d'oxyfluorure de silicium à dopage O2 est de préférence caractérisé par un contenu d'hydrogène moléculaire inférieur à 1x1017 molécules/cm3 d'hydrogène moléculaire ainsi que de faibles taux de chlore.
EP02714956A 2001-02-24 2002-02-11 Dopage a l'oxygene de verre d'oxyfluorure de silicium Withdrawn EP1373151A1 (fr)

Applications Claiming Priority (5)

Application Number Priority Date Filing Date Title
US27113501P 2001-02-24 2001-02-24
US271135P 2001-02-24
US09/997,782 US6502426B2 (en) 2001-02-24 2001-11-28 Oxygen doping of silicon oxyfluoride glass
US997782 2001-11-28
PCT/US2002/005237 WO2002068350A1 (fr) 2001-02-24 2002-02-11 Dopage a l'oxygene de verre d'oxyfluorure de silicium

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JP2009203142A (ja) * 2008-02-29 2009-09-10 Sumitomo Electric Ind Ltd フッ素添加石英ガラス
JP6702268B2 (ja) * 2017-06-15 2020-05-27 信越半導体株式会社 エピタキシャルウェーハの製造方法

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US3661436A (en) * 1970-06-30 1972-05-09 Ibm Transparent fabrication masks utilizing masking material selected from the group consisting of spinels, perovskites, garnets, fluorides and oxy-fluorides
JPH03131544A (ja) * 1989-06-29 1991-06-05 Sumitomo Electric Ind Ltd 光ファイバ用ガラス母材の加熱炉および製法

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