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WO2009004852A1 - Procédé d'élimination d'une matière étrangère à partir de la surface d'un substrat de verre et procédé de traitement d'une surface de substrat de verre - Google Patents

Procédé d'élimination d'une matière étrangère à partir de la surface d'un substrat de verre et procédé de traitement d'une surface de substrat de verre Download PDF

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Publication number
WO2009004852A1
WO2009004852A1 PCT/JP2008/057553 JP2008057553W WO2009004852A1 WO 2009004852 A1 WO2009004852 A1 WO 2009004852A1 JP 2008057553 W JP2008057553 W JP 2008057553W WO 2009004852 A1 WO2009004852 A1 WO 2009004852A1
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WO
WIPO (PCT)
Prior art keywords
glass substrate
processing
substrate surface
gas
mixed gas
Prior art date
Application number
PCT/JP2008/057553
Other languages
English (en)
Inventor
Masabumi Ito
Kenji Okamura
Hiroshi Kojima
Original Assignee
Asahi Glass Co., Ltd.
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
Application filed by Asahi Glass Co., Ltd. filed Critical Asahi Glass Co., Ltd.
Priority to EP08740610A priority Critical patent/EP2170778A1/fr
Priority to CN200880022677A priority patent/CN101687696A/zh
Publication of WO2009004852A1 publication Critical patent/WO2009004852A1/fr
Priority to US12/648,481 priority patent/US20100101940A1/en

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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
    • C03C15/00—Surface treatment of glass, not in the form of fibres or filaments, by etching
    • C03C15/02—Surface treatment of glass, not in the form of fibres or filaments, by etching for making a smooth surface
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y10/00—Nanotechnology for information processing, storage or transmission, e.g. quantum computing or single electron logic
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y40/00—Manufacture or treatment of nanostructures
    • 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
    • C03C15/00—Surface treatment of glass, not in the form of fibres or filaments, by etching
    • 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
    • C03C23/00—Other surface treatment of glass not in the form of fibres or filaments
    • 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
    • C03C23/00—Other surface treatment of glass not in the form of fibres or filaments
    • C03C23/0005—Other surface treatment of glass not in the form of fibres or filaments by irradiation
    • C03C23/0025—Other surface treatment of glass not in the form of fibres or filaments by irradiation by a laser beam
    • 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
    • C03C23/00—Other surface treatment of glass not in the form of fibres or filaments
    • C03C23/0005—Other surface treatment of glass not in the form of fibres or filaments by irradiation
    • C03C23/006—Other surface treatment of glass not in the form of fibres or filaments by irradiation by plasma or corona discharge
    • 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
    • C03C23/00—Other surface treatment of glass not in the form of fibres or filaments
    • C03C23/0075—Cleaning of 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
    • G03F1/22—Masks or mask blanks for imaging by radiation of 100nm or shorter wavelength, e.g. X-ray masks, extreme ultraviolet [EUV] masks; Preparation thereof
    • G03F1/24—Reflection masks; Preparation thereof
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
    • 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
    • G03F1/68—Preparation processes not covered by groups G03F1/20 - G03F1/50
    • G03F1/82—Auxiliary processes, e.g. cleaning or inspecting
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J2237/00—Discharge tubes exposing object to beam, e.g. for analysis treatment, etching, imaging
    • H01J2237/06—Sources
    • H01J2237/08—Ion sources
    • H01J2237/0812—Ionized cluster beam [ICB] sources
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J2237/00—Discharge tubes exposing object to beam, e.g. for analysis treatment, etching, imaging
    • H01J2237/30—Electron or ion beam tubes for processing objects
    • H01J2237/31—Processing objects on a macro-scale
    • H01J2237/3151—Etching

Definitions

  • the present invention relates to a method for removing foreign matter from a glass substrate surface and, in particular, to a method for removing foreign matter from a glass substrate surface which is required to have a high flatness, such as glass substrates to be used for a reflective type mask for EUV (extreme ultraviolet) lithography in the semiconductor manufacturing process. More specifically, the invention relates to a method for removing foreign matter from a glass substrate surface to be processed by a method accompanied with beam irradiation or laser light irradiation on a glass substrate surface, such as ion beam etching, gas cluster ion beam etching, plasma etching and nano-abrasion by means of laser light irradiation.
  • the invention relates to a method comprising removing foreign matter from a glass substrate surface, and then processing the glass substrate surface by a method accompanied with beam irradiation or laser light irradiation on the glass substrate surface, such as ion beam etching, gas cluster ion beam etching, plasma etching and nano-abrasion by means of laser light irradiation.
  • an exposure tool for manufacturing an integrated circuit by transferring a fine circuit pattern onto a wafer has hitherto been widely utilized.
  • the exposure tool is required to achieve image formation of a circuit pattern on a wafer surface with high resolution and a long focal depth, and shortening of the wavelength of an exposure light source is being advanced.
  • the exposure light source is further advancing from conventional g-rays (wavelength: 436 nm) , i-rays (wavelength: 365 nm) and a KrF excimer laser (wavelength: 248 nm) , and an ArF excimer laser (wavelength: 193 nm) is started to be used.
  • conventional g-rays wavelength: 436 nm
  • i-rays wavelength: 365 nm
  • a KrF excimer laser wavelength: 248 nm
  • an ArF excimer laser wavelength: 193 nm
  • the use of an F 2 laser (wavelength: 157 nm) as an exposure light source is regarded as promising. However, it is considered that even this is able to cover only the generation with a line width of up to 70 nm.
  • the EUV light refers to light of a waveband of a soft X-ray region or vacuum ultraviolet region, and specifically means light having a wavelength of from about 0.2 to 100 nm.
  • the exposure principle of this EUV lithography (hereinafter abbreviated as ⁇ ⁇ UVL") is identical with the conventional lithography in respect of transferring a mask pattern using a projection optical system.
  • ⁇ ⁇ UVL The exposure principle of this EUV lithography
  • the mask to be used for EUVL is basically configured of (1) a glass substrate, (2) a reflective multilayer film formed on the glass substrate and (3) an absorber layer formed on the reflective multilayer film.
  • the reflective multilayer film one having a structure in which plural materials having a different refractive index against the wavelength of the exposure light are cyclically laminated at a nanometer scale is used, and Mo and Si are known as representative materials.
  • Ta and Cr has been investigated as the material for the absorber layer.
  • As the glass substrate in order that a strain may not be generated even upon irradiation with EUV light, a material having a low heat expansion coefficient is required, and the use of a glass having a low heat expansion coefficient or a crystallized glass having a low heat expansion coefficient has been investigated. In this specification, the glass having a low heat expansion coefficient and the crystallized glass having a low heat expansion coefficient are collectively called "low expansion glass” or "ultra-low expansion glass”.
  • a quartz glass mainly composed of SiO 2 and to which TiO 2 , SnO 2 or ZrO 2 is added as a dopant for the purpose of reducing the heat expansion coefficient of glass is most widely used.
  • the glass substrate is manufactured by processing a raw material of such a glass or crystallized glass in high precision and washing it.
  • the glass substrate surface is pre-polished at a relatively high processing rate until it comes to have predetermined flatness and surface roughness; foreign matter such as a polishing waste generated by pre-polishing is removed by washing; and the glass substrate surface is then finish-processed by a method with higher processing precision so as to have desired flatness and surface roughness.
  • a method accompanied with beam irradiation or laser light irradiation on a glass substrate surface such as ion beam etching, gas cluster ion beam etching, plasma etching and nano-abrasion by means of laser light irradiation, is preferably used.
  • Patent Document 1 JP-T-2003-505891 DISCLOSURE OF THE INVENTION
  • an object of the invention is to provide a method for removing foreign matter from a glass substrate surface to be finish-processed by a method accompanied with beam irradiation or laser light irradiation on the glass substrate surface, such as ion beam etching, gas cluster ion beam etching, plasma etching and nano-abrasion by means of laser light irradiation.
  • Another object of the invention is to provide a method in which after removing foreign matter from a glass substrate surface, the glass substrate surface is processed by a method accompanied with beam irradiation or laser light irradiation on a glass substrate surface, such as ion beam etching, gas cluster ion beam etching, plasma etching and nano-abrasion by means of laser light irradiation.
  • the invention is to provide a method for removing foreign matter from a glass substrate surface, which comprises subjecting the glass substrate surface to gas cluster ion beam etching at an accelerating voltage of from 5 to 15 keV.
  • the invention is to provide a method for removing foreign matter from a glass substrate surface, which comprises subjecting the glass substrate surface to gas cluster ion beam etching with, as a gas source, at least one gas selected from the group consisting of O 2 , Ar, B, CO2, N 2 , N 2 O and a boron hydride.
  • the gas cluster ion beam etching is performed under a condition that the etching amount is not more than 20 nm.
  • the glass substrate is made of a low expansion glass having a heat expansion coefficient at 20 °C or at from 50 to 80 0 C of 0 ⁇ 30 ppb/°C .
  • the glass substrate surface before performing the gas cluster ion beam etching has a surface roughness (Rms) of not more than 5 nm.
  • the gas cluster ion beam etching is performed under a condition that a cluster size is 2, 000 or more. In the foreign matter removal method of the invention, it is preferable that the gas cluster ion beam etching is performed while keeping an angle formed by a normal line of the glass substrate and a gas cluster ion beam to be made incident to the glass substrate surface at from 3 to 60 degrees.
  • the gas cluster ion beam etching is performed while keeping the glass substrate surface in a state facing downward relative to the horizontal direction by from 3 to 60 degrees.
  • the invention is to provide a method for processing a glass substrate surface, which comprises the steps of: removing foreign matter on the glass substrate surface by the foreign matter removal method of the invention; and processing the glass substrate surface by a processing method selected from the group consisting of ion beam etching, gas cluster ion beam etching, plasma etching and nano-abrasion (this method will be hereinafter referred to as "processing method (1) of the invention") .
  • the processing method is gas cluster ion beam etching.
  • the gas cluster ion beam etching in the processing step is performed at an accelerating voltage exceeding 15 keV, using, as a source gas, a mixed gas selected from the group consisting of: a mixed gas of SF 6 and O 2 ; a mixed gas of SF 6 , Ar and O 2 ; a mixed gas of NF 3 and O 2 ; a mixed gas of NF 3 , Ar and O 2 ; a mixed gas of NF 3 and N 2 ; and a mixed gas of NF 3 , Ar and N 2 .
  • the source gas is any one mixed gas selected from the group consisting of: a mixed gas of SF 6 and O 2 ; a mixed gas of SF 6 , Ar and O 2 ; a mixed gas of NF 3 and O 2 ; and a mixed gas of NF 3 , Ar and O 2 .
  • the invention is to provide a method for processing a glass substrate surface, which comprises the steps of: measuring a flatness of the glass substrate surface; removing foreign matter on the glass substrate surface by the foreign matter removal method of the invention; and processing the glass substrate surface by a processing method selected from the group consisting of ion beam etching, gas cluster ion beam etching, plasma etching and nano-abrasion, wherein, in the step of processing the glass substrate surface, a processing condition of the glass substrate surface is set up for each site of the glass substrate on the basis of a result obtained from the step of measuring a flatness (this method will be hereinafter referred to as "processing method (2) of the invention”) .
  • the processing method is ion beam etching, gas cluster ion beam etching or plasma etching; a width of waviness existing on the glass substrate surface is specified on the basis of a result obtained from the step of measuring a flatness of the glass substrate surface; and the glass substrate surface is processed with a beam having a beam diameter of not more than the width of the waviness in terms of FWHM (full width of half maximum) value.
  • the FWHM value of the beam diameter is not more than 1/2 of the width of the waviness .
  • the processing method is gas cluster beam etching; and the gas cluster ion beam etching in the processing step is performed at an accelerating voltage exceeding 15 keV, using, as a source gas, a mixed gas selected from the group consisting of: any one mixed gas of SF 6 and O 2 ; a mixed gas of SF 6 , Ar and O 2 ; a mixed gas of NF 3 and O 2 ; a mixed gas of NF 3 , Ar and O2; a mixed gas of NF 3 and N2; and a mixed gas of NF 3 , Ar and N 2 .
  • a mixed gas selected from the group consisting of: any one mixed gas of SF 6 and O 2 ; a mixed gas of SF 6 , Ar and O 2 ; a mixed gas of NF 3 and O 2 ; a mixed gas of NF 3 , Ar and O2; a mixed gas of NF 3 and N2; and a mixed gas of NF 3 , Ar and N 2 .
  • the source gas is any one mixed gas selected from the group consisting of: a mixed gas of SF 6 and O 2 ; a mixed gas of SF 6 , Ar and O 2 ; a mixed gas of NF 3 and O 2 ; and a mixed gas of NF 3 , Ar and O 2 .
  • a second processing step is performed for improving a surface roughness of the glass substrate surface.
  • gas cluster ion beam etching is performed at an accelerating voltage of 3 keV or more and less than 30 keV, using, as a source gas, an O 2 gas singly or a mixed gas of O 2 and at least one gas selected from the group consisting of Ar, CO and CO 2 .
  • mechanical polishing using a polishing slurry is performed at a surface pressure of from 1 to 60 gf/cm 2 .
  • the invention is to provide a glass substrate obtained by the processing method of the invention, wherein the substrate surface has a flatness of not more than 50 nm, and is free from a convex glass defect having a height exceeding 1.5 nm.
  • a glass substrate surface is finish-processed by a method accompanied with beam irradiation or laser light irradiation on the glass substrate surface, such as ion beam etching, gas cluster ion beam etching, plasma etching and nano-abrasion by means of laser light irradiation, it is possible to prevent the generation of a convex defect of the glass on the glass substrate surface after processing and to process the glass substrate surface into a surface having excellent flatness and surface roughness.
  • Fig. 1 is a schematic view illustrating the relationship between a processing surface of a substrate and GCIB in the foreign matter removal method of the invention.
  • the foreign matter removal method of the invention is concerned with a method for removing foreign matter from a glass substrate surface to be finish-processed (this glass substrate surface will be also referred to as "processing surface") , namely the processing surface before finish-processing, by a method accompanied with beam irradiation or laser light irradiation on a glass substrate surface, such as ion beam etching, gas cluster ion beam etching, plasma etching and nano-abrasion by means of laser light irradiation.
  • Such a processing surface is washed before performing the finish-processing. On that occasion, there is the case where foreign matter which has not been completely removed by washing remains; or the case where foreign matter newly attaches onto the glass substrate surface after washing.
  • the foreign matter removal method of the invention is aimed to remove such foreign matter.
  • the foreign matter which is a target of the foreign matter removal method of the invention refers to a material attaching onto the processing surface by a van der Waals force but not a material fixing onto the processing surface by a chemical bond, and its size is usually from about 1 to 2 ⁇ m or smaller.
  • the glass substrate which is a target of the foreign matter removal method of the invention is a glass substrate for a reflective type mask for EUVL capable of mainly coping with higher integration and higher definition of an integrated circuit.
  • the glass substrate to be used for this application is a glass substrate having a small heat expansion coefficient and a small scattering thereof.
  • the glass substrate is preferably- made of a low expansion glass having a heat expansion coefficient at 20 °C or at from 50 to 80 0 C of 0 ⁇ 30 ppb/°C, and more preferably made of an ultra-low expansion glass having a heat expansion coefficient at 20 °C or at from 50 to 80 0 C of 0 ⁇ 10 ppb/°C.
  • the glass substrate is not particularly limited with respect to the shape, size and thickness and the like.
  • a substrate for a reflective type mask for EUVL its shape is a rectangular plate-shaped body in view of a rectangular planar shape.
  • the processing surface is preliminarily processed so as to have predetermined flatness and surface roughness .
  • the foreign matter removal method of the invention which is described below in detail, is a method for removing foreign matter existing on the processing surface without substantially processing the processing surface. For that reason, it is preferable that prior to performing the foreign matter removal method of the invention, the processing surface is preliminarily processed so as to have predetermined flatness and surface roughness by a processing method having a relatively high processing rate.
  • the processing method to be used for the preliminary processing is not particularly limited but can be widely chosen among known processing methods to be used for processing a glass surface.
  • a mechanical polishing method is usually used.
  • the mechanical polishing method as referred to herein includes, in addition to polishing processing only by means of a polishing function with an abrasive grain, a method of using a polishing slurry which utilizes a polishing function with an abrasive grain and a chemical polishing function with a chemical in combination.
  • the mechanical polishing method may be any of lapping and polishing, and a polishing tool and an abrasive to be used can be appropriately chosen from known ones.
  • a polishing tool and an abrasive to be used can be appropriately chosen from known ones.
  • the mechanical polishing method for the purpose of making the processing rate large, it is preferable in the case of lapping that the lapping is performed at a surface pressure of from 30 to 70 gf/cm 2 , and more preferably at a surface pressure of from 40 to 60 gf/cm 2 ; whereas it is preferable in the case of polishing that the polishing is performed at a surface pressure of from 60 to 140 gf/cm 2 , and more preferably at a surface pressure of from 80 to 120 gf/cm 2 .
  • the lapping is preferably performed so as to give a lapping amount of from 100 to 300 ⁇ m, and the polishing is preferably performed so as to give a polishing amount of from 1 to 60 ⁇ m.
  • the processing surface after the preliminary processing preferably has a surface roughness (Rms) of not more than 5 run, and more preferably not more than 1 run.
  • the surface roughness as referred to in this specification means a surface roughness measured by an atomic force microscope with respect to an area of from 1 to 10 ⁇ m square.
  • the foreign matter removal method of the invention is characterized in that by performing gas cluster ion beam (hereinafter referred to as "GCIB”) etching under a specified condition that gives a low etching amount with respect to the processing surface (this condition will be hereinafter referred to as “low etching condition”) , foreign matter is removed from the processing surface while making the processing amount of the processing surface extremely low.
  • GCIB gas cluster ion beam
  • the GCIB etching as referred to herein is a method in which a reactive substance (source gas) which is in a gaseous state at normal temperature and atmospheric pressure is jetted in a pressurized state into a vacuum apparatus via an expansion type nozzle to form a gas cluster, which is then ionized upon irradiation with an electron, and the resulting GCIB is irradiated on a target to achieve etching.
  • the gas cluster is usually constituted of a massive atomic group or molecular group composed of several thousand atoms or molecules.
  • the processing surface by performing the GCIB etching on the processing surface, when the gas cluster comes into collision with the processing surface, a multiple collision effect is generated due to a mutual action with the solid, whereby the foreign matter is removed from the processing surface. Then, since GCIB etching is performed on the processing surface under a low etching condition, the processing surface is not substantially processed.
  • the GCIB etching may be selectively performed in this site.
  • a method of scanning GCIB luster scanning and spiral scanning are known, and any of these methods may be used.
  • an accelerating voltage for applying to accelerating electrodes is controlled at from 5 to 15 keV.
  • the source gas which is used in performing the GCIB etching for the purpose of finish-processing the glass substrate surface may be a conventionally used source gas.
  • a conventional source gas include SF 6 , NF 3 , CHF 3 , CF 4 , C 2 F 6 , C 3 F 8 , C 4 F 6 , SiF 4 and COF 2 . These gases may be used singly or in admixture.
  • the etching amount on the processing surface is sufficiently low, and foreign matter existing on the processing surface can be removed without substantially processing the processing surface.
  • the accelerating voltage is less than 5 keV, when the gas cluster comes into collision with the processing surface, the kinetic energy is small so that foreign matter existing on the processing surface cannot be removed depending upon the size of the foreign matter. Specifically, foreign matter having a size of from about 1 to 2 ⁇ m cannot be removed.
  • the accelerating voltage is more preferably from 5 to 10 keV.
  • the GCIB etching is performed using, as a gas source, at least one gas selected from O 2 , Ar, B, CO2, N 2 O and a boron hydride (for example, BH 3 and B 4 Hi 0 ) •
  • a gas species for example, BH 3 and B 4 Hi 0
  • the GCIB etching is performed using such a gas species as the source gas, foreign matter existing on the processing surface can be removed without substantially processing the processing surface.
  • the accelerating voltage for applying a gas species having an extremely weak etching action to accelerating electrodes is not particularly limited.
  • the accelerating voltage is more preferably 20 keV or more, and further preferably 30 keV or more.
  • the accelerating voltage is less than 15 keV, when the gas cluster comes into collision with the processing surface, the kinetic energy is small, and therefore, there is a possibility that foreign matter existing on the processing surface cannot be removed depending upon the size of the foreign matter.
  • the accelerating voltage is less than 15 keV, by adjusting the cluster size, dose amount, irradiation time and the like, foreign matter existing on the processing surface can be removed.
  • the low etching condition as referred to herein is preferably a condition under which the etching amount is not more than 20 run, and more preferably a condition under which the etching amount is not more than 10 nm.
  • the irradiation condition for example, a cluster size, an ionizing current to be applied to ionization electrodes of a GCIB etching apparatus for ionizing the cluster and a dose amount of GCIB can be appropriately chosen in accordance with the kind of a source gas, the accelerating voltage to be applied to accelerating electrodes and the like. It is preferable that the GCIB etching is performed under a condition that a cluster size is 2,000 or more. When the cluster size is 2,000 or more, since a relatively large gas cluster comes into collision with the processing surface, it is expected that an effect for removing foreign matter existing on the processing surface is enhanced due to the multiple collision effect.
  • the cluster size is more preferably 3,000 or more, and especially preferably 5,000 or more.
  • Fig. 1 is a view illustrating the state that GCIB is irradiated on a processing surface from an oblique direction thereto.
  • a normal line N of a glass substrate 1 (accordingly, a normal line N of a processing surface 10) and GCIB to be made incident to the processing surface 10 is kept at from
  • the angle ⁇ is kept more preferably at from 10 to 60 degrees, and further preferably at from 30 to 60 degrees.
  • GCIB is irradiated on the processing surface from an oblique direction thereto, as illustrated in Fig. 1, it is preferable that GCIB is irradiated in a horizontal direction in a state that the processing surface 10 faces downward relative to the horizontal direction by from 3 to 60 degrees. According to this, not only an effect for removing foreign matter existing on the processing surface is enhanced due to the multiple collision effect, but it is possible to prevent the removed foreign matter from the reattachment onto the processing surface.
  • the processing surface 10 is kept in a state facing downward relative to the horizontal direction preferably by from 10 to 60 degrees, and more preferably by from 30 to 60 degrees.
  • the processing method (1) of the invention includes a step of removing foreign matter on a glass substrate surface by the foregoing foreign matter removal method of the invention (this step will be hereinafter referred to as “foreign matter removal step”) ; and a step of processing the glass substrate surface by a processing method selected from the group consisting of ion beam etching, GCIB etching, plasma etching and nano-abrasion (this step will be hereinafter referred to as "processing step”) .
  • the processing surface is pre- polished so as to have predetermined flatness and surface roughness
  • the processing surface is finish- processed by a processing method selected from the group consisting of ion beam etching, GCIB etching, plasma etching and nano-abrasion.
  • the foreign matter removal step and the processing step are performed in the same chamber or performed in chambers placed side by side in such a manner that the substrate can be conveyed without being discharged from the apparatus.
  • GCIB etching it is preferable to use the same GCIB etching apparatus in the foreign matter removal step and the processing step.
  • GCIB etching because the surface can be processed so as to have a small surface roughness and excellent smoothness.
  • a gas such as SF 6 , Ar, O 2 , N 2 , NF 3 , N 2 O, CHF 3 , CF 4 , C 2 F 6 , C 3 F 8 , C 4 F 6 , SiF 4 and COF 2 can be used singly or in admixture as a source gas.
  • SF 6 , NF 3 , CHF 3 , CF 4 , C 2 F 6 , C 3 F 8 , C 4 F 6 , SiF 4 and COF 2 are excellent as the source gas from the standpoint of a chemical reaction which occurs when the gas cluster comes into collision with the processing surface.
  • mixed gases containing SF 6 or NF 3 specifically a mixed gas of SF 6 and O 2 , a mixed gas of SF 6 , Ar and O 2 , a mixed gas of NF 3 and O 2 , a mixed gas of NF 3 , Ar and O 2 , a mixed gas of NF 3 and N 2 and a mixed gas of NF 3 , Ar and N 2 are preferable for reasons that the etching rate is high and that the processing tact is enhanced.
  • a mixed gas though a favorable mixing ratio of the respective components varies with a condition such as an irradiation condition, the following are preferable.
  • SF 6 /O 2 0.1 to 5 %/95 to 99.9 % (a mixed gas of SF 6 and O 2 )
  • SF 6 /Ar/O 2 0.1 to 5 %/9.9 to 49.9 %/50 to 90 % (a mixed gas of SF 6 , Ar and O 2 )
  • NF 3 /O 2 0.1 to 5 %/95 to 99.9 % (a mixed gas of NF 3 and O 2 )
  • NF 3 /Ar/O 2 0.1 to 5 %/9.9 to 49.9 %/50 to 90 % (a mixed gas of NF 3 , Ar and O 2 )
  • NF 3 /N 2 0.1 to 5 %/95 to 99.9 % (a mixed gas of NF 3 and N 2 )
  • NF 3 /Ar/N 2 0.1 to 5 %/9.9 to 49.9 %/50 to 90 % (a mixed gas of NF 3 , Ar and N 2 )
  • a mixed gas of SF 6 and O 2 a mixed gas of SF 6 , Ar and O 2 , a mixed gas of NF 3 and O 2 and a mixed gas of NF 3 , Ar and O 2 are preferable.
  • the irradiation condition for example, a cluster size, an ionizing current to be applied to ionization electrodes of a GCIB etching apparatus for ionizing the cluster and a dose amount of GCIB can be appropriately chosen in accordance with the kind of the source gas, the surface properties of the processing surface, the purpose of finish-processing and the like.
  • the accelerating voltage to be applied to accelerating electrodes exceeds 15 keV; and for the purpose of improving the flatness of the processing surface without excessively deteriorating the surface roughness, it is preferable that the accelerating voltage exceeds 15 keV and is not more than 30 keV.
  • the processing method (2) of the invention includes a step of measuring a flatness of a glass substrate surface (this step will be hereinafter referred to as "flatness measuring step”) ; a step of removing foreign matter on the processing surface by the foregoing foreign matter removal method of the invention (this step will be hereinafter referred to as “foreign matter removal step”) ; and a step of processing the processing surface by a processing method selected from the group consisting of ion beam etching, GCIB etching, plasma etching and nano- abrasion (this step will be hereinafter referred to as "processing step”) , wherein in the processing step, a processing condition of the processing surface is set up for each site of the processing surface on the basis of a result obtained from the flatness measuring
  • waviness means irregularities having a cycle of from 5 to 30 mm among cyclic irregularities existing on the processing surface .
  • the processing method (2) of the invention is a method in which such waviness generated on the processing surface after the preliminary processing is removed, and the processing surface is finish-processed into a surface with excellent flatness.
  • the flatness measuring step is performed prior to the processing step.
  • the flatness measuring step may be performed after the foreign matter removal step. However, in order to prevent the attachment of a new foreign matter onto the processing surface after the foreign matter removal step, it is preferable that the flatness measuring step is performed prior to the foreign matter removal step.
  • the foreign matter removal step and the processing step are performed in the same chamber or performed in chambers placed side by side in such a manner that the substrate can be conveyed without being discharged from the apparatus.
  • GCIB etching it is preferable to use the same GCIB etching apparatus in the foreign matter removal step and the processing step.
  • the flatness in each site of the processing surface namely a difference of altitude is measured. Accordingly, the result obtained from the flatness measuring step becomes a flatness map showing a difference of altitude in each site of the processing surface (this will be hereinafter referred to as "flatness map") .
  • the flatness in each site of the processing surface can be, for example, measured by a laser interference type flatness measuring device. However, it should not be construed that the invention is limited thereto.
  • the flatness map may be prepared using a measurement result obtained by measuring a difference of altitude in each site of the processing surface using a laser displacement gauge, an ultrasonic displacement gauge or a contact type displacement gauge.
  • the processing condition of the processing surface is set up for each site of the processing surface on the basis of a result obtained from the flatness measuring step.
  • the result obtained from the flatness measuring step becomes a flatness map.
  • the flatness map is expressed by S (x, y) ( ⁇ m) .
  • the processing time is expressed by T (x, y) (min) .
  • the processing rate is defined as Y ( ⁇ m/min) , the relationship of these is expressed by the following equation.
  • the processing condition of the processing surface is set up for each site of the processing surface on the basis of a result obtained from the flatness measuring step
  • the processing condition specifically the processing time is set up for each site of the processing surface according to the foregoing equation.
  • the processing condition of the processing surface can be set up for each site of the processing surface on the basis of a result obtained from the flatness measuring step.
  • a setup procedure for this is hereunder specifically described.
  • the width of the waviness existing on the processing surface is specified using a result obtained from the flatness measuring step.
  • the width of the waviness as referred to herein means a length of a concave portion or a convex portion in the convex-concave shape existing cyclically on the processing surface. Accordingly, the width of the waviness is usually 1/2 of a cycle of the width of the waviness. In the case where a plural number of waviness having different cycles exit, the width of the waviness having the smallest cycle is taken as the width of the waviness existing on the processing surface.
  • the measurement result obtained from the flatness measuring step is a flatness map showing a difference of altitude in each site of the processing surface. Accordingly, it is possible to easily specify the width of the waviness existing on the processing surface from the flatness map.
  • Ion beam etching, GCIB etching or plasma etching is performed with a beam having a beam diameter of not more than the width of the waviness on the basis of the width of the waviness as specified in the foregoing procedure.
  • the beam diameter as referred to herein is based on FWHM (full width of half maximum) value. In this specification, when the beam diameter is referred to, it means the FWHM value of the beam diameter.
  • the processing step when a method accompanied with the beam irradiation on the processing surface is used, namely in the case of using ion beam etching, GCIB etching or plasma etching, it is necessary that a beam is scanned on the processing surface. This is because in order to set up a processing condition of the processing surface for each site of the processing surface, it is required to make the range to be irradiated with a beam at one time small as far as possible. In particular, in the case of using a beam having a beam diameter of not more than the width of the waviness, it is necessary to scan the processing surface with the beam. As a method of scanning with a beam, luster scanning and spiral scanning are known, and any of these methods may be used.
  • GCIB etching because the surface can be processed so as to have a small surface roughness and excellent smoothness.
  • the source gas and irradiation condition are the same as those described regarding the processing method (1) of the invention.
  • first processing step a second processing step for the purpose of improving the surface roughness of the processing surface is performed.
  • GCIB etching can be used.
  • the GCIB etching is performed by changing an irradiation condition such as a source gas, an ionizing current and an accelerating voltage from those used in the GCIB etching to be used in the foreign matter removal method and the GCIB etching to be used in the first processing step.
  • the GCIB etching is performed under an irradiation condition such that the etching amount is lower than that in the GCIB etching to be used in the first processing step.
  • the GCIB etching is performed under a more gentle condition using a lower ionizing current or a lower accelerating voltage.
  • the accelerating voltage is preferably 3 keV or more and less than 30 keV, and more preferably from 3 to 20 keV.
  • a source gas an O 2 gas singly or a mixed gas of O 2 and at least one gas selected from the group consisting of Ar, CO and CO 2 from the standpoint that when the source gas comes into collision with the processing surface, it hardly causes a chemical reaction.
  • a mixed gas of O 2 and Ar it is preferable to use a mixed gas of O 2 and Ar.
  • mechanical polishing using a polishing slurry which is called touch polishing
  • a glass substrate is set interposed between polishing plates each provided with a polishing pad made of a non-woven fabric, a woven fabric or the like, and the polishing plates are relatively rotated against the glass substrate while feeding a slurry adjusted so as to have predetermined properties, thereby polishing processing the processing surface at a surface pressure of from 1 to 60 gf/cm 2 .
  • polishing pad for example, BELLATRIX K7512, manufactured by Kanebo, Ltd. is useful.
  • the polishing slurry it is preferable to use a colloidal silica- containing polishing slurry; and it is more preferable to use a polishing slurry containing colloidal silica having an average primary particle size of not more than 50 nm and water and adjusted so as to have a pH in the range of from 0.5 to 4.
  • the surface pressure of polishing is from 1 to 60 gf/cm 2 . When the surface pressure exceeds 60 gf/cm 2 , it is impossible to process the processing surface to a desired surface roughness due to the generation of a scratch scar on the substrate surface or the like.
  • the surface pressure is less than 1 gf/cm 2 , it takes a long period of time for the processing, and hence, such is not practically useful. Also, when the surface pressure is less than 30 gf/cm 2 , it takes a long period of time for the processing. Therefore, it is preferable that after processing at a surface pressure of from 30 to 60 gf/cm 2 to some extent, the surface is finish-processed at a surface pressure of from 1 to 30 gf/cm 2 .
  • the average primary particle size of colloidal silica is preferably less than 20 nm, more preferably less than 15 nm, and especially preferably less than 10 nm.
  • the average primary particle size of colloidal silica exceeds 50 nm, it is difficult to process the processing surface so as to have a desired surface roughness.
  • its average particle size is preferably not more than 70 nm.
  • the particle size of colloidal silica as referred to herein is a particle size obtained by measuring an image with a magnification of from 15 to 105 x 10 3 times by SEM (scanning electron microscope) .
  • the content of colloidal silica in the polishing slurry is preferably from 10 to 30 % by mass.
  • the content of colloidal silica in the polishing slurry is less than 10 % by mass, there is a possibility that the polishing efficiency may become worse, whereby economic polishing is not attained.
  • the content of colloidal silica exceeds 30 % by mass, since the use amount of colloidal silica increases, there is a possibility of causing a trouble from the viewpoints of costs and washability.
  • the content of colloidal silica in the polishing slurry is more preferably from 18 to 25 % by mass, and especially preferably from 18 to 22 % by mass.
  • the pH of the polishing slurry is made to fall within the foregoing acidic range, namely the pH is made to fall within the range of from 0.5 to 4, it is possible to subject the processing surface to chemical and mechanical polishing processing, thereby achieving efficient polishing processing of the processing surface with good smoothness. That is, the convex portions of the processing surface are softened by an acid of the polishing slurry, and therefore, the convex portions can be easily removed by mechanical polishing. According to this, not only the processing efficiency is enhanced, but a glass waste which has been removed off by the polishing processing is softened, and therefore, the generation of a new damage due to the glass waste or the like is prevented.
  • the pH of the polishing slurry is less than 0.5, there is a possibility that corrosion is generated in a polishing machine to be used for touch polishing.
  • the pH is preferably 1 or more.
  • the pH is preferably not more than 4, and especially preferably in the range of from 1.8 to 2.5.
  • the pH adjustment of the polishing slurry can be achieved by adding an inorganic acid or an organic acid singly or a combination thereof.
  • the inorganic acid which can be used include nitric acid, sulfuric acid, hydrochloric acid, perchloric acid and phosphoric acid. Of these, nitric acid is preferable in view of easiness of handling.
  • examples of the organic acid include oxalic acid and citric acid.
  • pure water or ultrapure water from which foreign matter has been removed is preferably used. That is, pure water or ultrapure water which substantially has not more than one fine particle having a maximum size, as measured by a light scattering mode using laser light or the like, of
  • 0.1 ⁇ m or more per mL is preferable.
  • the foreign matter in pure water or ultrapure water can be removed by, for example, filtration or ultrafiltration with a membrane filter, but it should not be construed that the removal method of foreign matter is limited thereto.
  • the processing surface has excellent flatness and surface roughness; the flatness of the processing surface after processing is not more than 50 run; and a convex defect of the glass having a height exceeding 1.5 nm does not exist on the processing surface.
  • the flatness of the processing surface after processing is more preferably not more than 30 nm, and further preferably not more than 20 nm.
  • the glass substrate as processed by the processing method of the invention is favorable as an optical device to be used in an optical system of an exposure tool for semiconductor manufacture, especially an optical device to be used in an optical system of a next-generation exposure tool for semiconductor manufacture with a line width of not more than 45 ran because the processing surface has excellent flatness and surface roughness.
  • an optical device include lenses, diffraction gratings, optical membrane bodies and composite bodies thereof, for example, lenses, multi- lenses, lens arrays, lenticular lenses, fly-eye lenses, aspheric lenses, mirrors, diffraction gratings, binary optics devices, photomasks and composite bodies thereof.
  • the glass substrate as processed by the processing method of the invention is favorable as a photomask and a mask blanks for manufacturing this photomask, especially a reflective type mask for EUVL and a mask blanks for manufacturing this mask.
  • the light source of the exposure tool is not particularly limited and may be a conventional laser capable of emitting g-rays (wavelength: 436 ran) or i-rays (wavelength: 365 ran) .
  • light sources of a shorter wavelength specifically light sources having a wavelength of not more than 250 run are preferable.
  • Specific examples of such a light source include a Kr F excimer laser (wavelength: 248 ran) , an ArF excimer laser (wavelength: 193 nm) , an F 2 laser (wavelength: 157 ran) and EUV (wavelength: 13.5 nm) .

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Abstract

L'invention a pour but de proposer un procédé pour éliminer une matière étrangère à partir d'une surface d'un substrat de verre devant être soumise à un traitement de finition par un procédé accompagné par une irradiation par un faisceau ou une irradiation par de la lumière laser sur la surface du substrat de verre. La présente invention porte sur un procédé pour éliminer la matière étrangère à partir d'une surface de substrat de verre qui comprend l'opération consistant à soumettre la surface de substrat de verre à une gravure par un faisceau d'amas gazeux ionisés à une tension d'accélération de 5 à 15 keV.
PCT/JP2008/057553 2007-06-29 2008-04-11 Procédé d'élimination d'une matière étrangère à partir de la surface d'un substrat de verre et procédé de traitement d'une surface de substrat de verre WO2009004852A1 (fr)

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EP08740610A EP2170778A1 (fr) 2007-06-29 2008-04-11 Procédé d'élimination d'une matière étrangère à partir de la surface d'un substrat de verre et procédé de traitement d'une surface de substrat de verre
CN200880022677A CN101687696A (zh) 2007-06-29 2008-04-11 从玻璃衬底表面除去杂质的方法和处理玻璃衬底表面的方法
US12/648,481 US20100101940A1 (en) 2007-06-29 2009-12-29 Method for removing foreign matter from glass substrate surface and method for processing glass substrate surface

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JP2007-172274 2007-06-29

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JP2009029691A (ja) 2009-02-12
CN101687696A (zh) 2010-03-31

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