WO2014050700A1 - ガラス再生処理方法および再生ガラス基板とそれを用いたフォトマスクブランクスとフォトマスク - Google Patents

ガラス再生処理方法および再生ガラス基板とそれを用いたフォトマスクブランクスとフォトマスク Download PDF

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Publication number
WO2014050700A1
WO2014050700A1 PCT/JP2013/075314 JP2013075314W WO2014050700A1 WO 2014050700 A1 WO2014050700 A1 WO 2014050700A1 JP 2013075314 W JP2013075314 W JP 2013075314W WO 2014050700 A1 WO2014050700 A1 WO 2014050700A1
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WIPO (PCT)
Prior art keywords
glass substrate
photomask
thin film
metal thin
pattern
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PCT/JP2013/075314
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English (en)
French (fr)
Japanese (ja)
Inventor
一樹 木下
悟 二嶋
陽祐 青木
敬二郎 板倉
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大日本印刷株式会社
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Application filed by 大日本印刷株式会社 filed Critical 大日本印刷株式会社
Priority to KR1020177031593A priority Critical patent/KR101963996B1/ko
Priority to JP2014538440A priority patent/JP6256344B2/ja
Priority to KR1020187034398A priority patent/KR102085058B1/ko
Priority to KR1020157005441A priority patent/KR101848983B1/ko
Priority to CN201380047359.8A priority patent/CN104620176B/zh
Publication of WO2014050700A1 publication Critical patent/WO2014050700A1/ja

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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B09—DISPOSAL OF SOLID WASTE; RECLAMATION OF CONTAMINATED SOIL
    • B09B—DISPOSAL OF SOLID WASTE NOT OTHERWISE PROVIDED FOR
    • B09B5/00—Operations not covered by a single other subclass or by a single other group in this subclass
    • 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
    • C03C17/00—Surface treatment of glass, not in the form of fibres or filaments, by coating
    • C03C17/22—Surface treatment of glass, not in the form of fibres or filaments, by coating with other inorganic material
    • 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
    • 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
    • C03C2218/00—Methods for coating glass
    • C03C2218/30—Aspects of methods for coating glass not covered above
    • C03C2218/32—After-treatment
    • C03C2218/328—Partly or completely removing a coating
    • C03C2218/33—Partly or completely removing a coating by etching
    • 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
    • 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
    • G03F1/72—Repair or correction of mask defects

Definitions

  • the present invention provides a new photomask which is patterned with a metal thin film and used as a photomask used in production in a photolithographic (hereinafter also referred to as photolithography) process of various flat panels or a photomask which has become defective in the photomask manufacturing process.
  • the present invention relates to a method for regenerating a glass substrate for reuse as a glass substrate, a photomask glass substrate regenerated by this regenerating method, a photomask blank and a photomask using the same.
  • Photomasks generally used in the manufacture of flat panels, etc. are made of photomask blanks in which a light-shielding layer is formed by laminating a metal thin film such as chromium, chromium oxide, or chromium nitride on a low expansion glass substrate such as synthetic quartz.
  • the photomask blank is formed by forming a pattern by EB drawing or laser drawing using a photolithography method.
  • Such a photomask is incorporated and used in various exposure apparatuses used to form pixels such as liquid crystal display devices, organic EL display devices, and high-precision touch panels. Synthetic quartz is used for the photomasks used in these products due to their quality performance.In recent years, with the increase in size of panels, the size of photomasks is increasing, and the glass substrates for photomasks are becoming more expensive. Reuse of used or defective photomasks has become an important technology.
  • the photomask substrate synthetic quartz is generally used as the material of the glass substrate for the photomask from the viewpoint of quality and accuracy, and the size of the glass substrate is the first generation substrate 320 mm ⁇ the flat panel substrate of the liquid crystal display device.
  • the photomask glass substrate size was 330 mm ⁇ 450 mm, which was slightly larger than the panel glass substrate, and the batch exposure was performed. Exposure methods such as exposure and feed methods such as step feed and scan method are diversified, and photomask sizes are becoming larger and more diversified.
  • the fifth generation of flat panel substrates is 1000 mm ⁇ 1200 mm, and the photomask substrate size is generally 520 mm ⁇ 800 mm or 800 mm ⁇ 920 mm.
  • the 8th generation flat panel substrate is 2160 mm ⁇ 2460 mm, and the photomask substrate size used therefor is 1220 mm ⁇ 1400 mm.
  • flat panels generally have one photo and one leaf, and each product has a different photomask pattern. These photomasks are not required when production of the product is completed.
  • the patterned metal thin film is dissolved and removed with an etching solution to form a bare glass.
  • the metal thin film pattern is formed in the used photomask substrate or the photomask process, the metal thin film pattern is dissolved and removed with an etching solution and washed again.
  • the substrate is patterned by photolithography, there is a problem that the original pattern remains and pattern defects are likely to occur.
  • an abrasive is further used to clean and homogenize the glass surface. Then, the glass surface was physically polished, washed to remove the polishing agent used for polishing, and reused as a glass substrate for a photomask.
  • Patent document 1 is a method for regenerating a substrate having a surface scratch on a photomask.
  • the scratch generated in the photomask manufacturing process is removed by dissolving the light shielding layer of the photomask to remove the glass substrate to the depth of the scratch. Grinding is used to remove scratches on the glass surface, and the surface with minute irregularities resulting from surface grinding is mirror-finished and polished to be regenerated into raw glass.
  • Patent Document 2 is a method for reclaiming a quartz jig used in a CVD process for semiconductor manufacturing.
  • An unnecessary deposited layer deposited on the surface of a quartz jig, an inner wall of a quartz tube, or the like is etched and washed with an HF aqueous solution.
  • the surface is smoothed by irradiating a rough quartz jig with light having a wavelength in the vacuum ultraviolet region, which is the same method for reclaiming quartz glass.
  • a conventional method for recycling a photomask glass substrate will be described with reference to FIG.
  • the patterned metal thin film is dissolved and removed with an etching solution to form a bare glass state (K1), and then the glass surface is made uniform by physical polishing with an abrasive such as cerium oxide. Polishing is performed using a polishing apparatus for rough polishing and a polishing apparatus for finishing surface polishing as the polishing apparatus (K2). Subsequently, cleaning is performed using an abrasive removal cleaning device and a finish cleaning device for removing the abrasive (K3), and then the appearance is inspected (K4) to produce a recycled substrate.
  • a waste disposal device for abrasives removed by cleaning is also required as an accessory device, which requires a high device price, wide installation space for the device, long processing time, and removal of foreign matter during polishing. Occurrence of scratches due to mixing and the flatness of the surface of the photomask may be disrupted, resulting in problems of production cost and production efficiency.
  • a glass substrate from which a metal thin film has been dissolved and removed is subjected to wet wettability homogenization treatment without physical polishing, thereby obtaining a regenerated substrate with low cost and few pattern defects.
  • the first of the gist of the present invention to solve the above problems is In the method for regenerating a glass substrate for a photomask having a pattern formed of a metal thin film on at least one surface, After dissolving and removing the metal thin film formed on the glass substrate with an etching solution, Performing wet wettability homogenization until the pattern does not appear in the breath image test, A method for regenerating a glass substrate for a photomask.
  • a second aspect of the present invention for solving the above problems is Repeatedly performing the wet wettability homogenization treatment and the breath image inspection;
  • the third of the gist of the present invention for solving the above problems is as follows.
  • the wet wettability homogenizing process is a process for homogenizing the wettability of the surface of the glass substrate for photomask, The method for regenerating a glass substrate for a photomask according to claim 1 or 2, wherein the glass substrate for photomask is reclaimed.
  • the fourth of the gist of the present invention for solving the above problems is as follows.
  • the wet wettability homogenization treatment is treatment with an alkaline aqueous solution,
  • the fifth of the gist of the present invention for solving the above problems is as follows.
  • the alkaline component of the alkaline aqueous solution is potassium hydroxide,
  • the sixth of the gist of the present invention for solving the above problems is as follows.
  • a glass substrate that has been regenerated from a photomask having a metal thin film pattern formed on at least one surface of the glass substrate In the glass substrate, a metal thin film formed as a photomask is dissolved and removed by an etching solution, A glass substrate for a photomask, characterized in that the wet wettability is uniformed so that the pattern does not appear in the breath image inspection.
  • the seventh of the gist of the present invention for solving the above problems is as follows.
  • the wet wettability homogenization process and the breath image inspection are repeatedly performed,
  • the eighth of the gist of the present invention for solving the above problems is
  • the wettability of the surface of the glass substrate for photomask is made uniform by the wet wettability homogenization treatment,
  • the ninth of the gist of the present invention for solving the above problems is as follows.
  • the wet wettability homogenization treatment is treated with an alkaline aqueous solution,
  • the glass substrate for a photomask according to any one of claims 6 to 8, wherein
  • the tenth aspect of the present invention for solving the above problems is as follows.
  • the alkaline component of the alkaline aqueous solution is potassium hydroxide,
  • the eleventh aspect of the present invention for solving the above problems is as follows.
  • the difference in the contact angle of water on the surface of the glass substrate for photomask that has been subjected to the regeneration treatment is 1 degree or less,
  • the twelfth aspect of the present invention for solving the above problems is Use of the glass substrate for a photomask according to any one of claims 6 to 11, A blank for photomasks.
  • the thirteenth aspect of the present invention for solving the above problems is Use of the blank for photomask according to claim 12; A photomask characterized by
  • the fourteenth aspect of the present invention for solving the above problems is From a photomask having a glass substrate and a metal thin film formed in a pattern on one surface of the glass substrate, a dissolution removal step of dissolving and removing the metal thin film using an etchant; A wet wettability homogenization treatment step of bringing an aqueous alkaline solution into contact with the surface of the glass substrate after the dissolution and removal step and performing wet wettability homogenization treatment; A method for producing a recycled glass substrate for a photomask, comprising:
  • the fifteenth aspect of the present invention for solving the above problems is In the above invention, the alkaline component of the alkaline aqueous solution is potassium hydroxide.
  • the sixteenth aspect of the present invention for solving the above problems is Regeneration in which wet wetting uniformity is performed until the pattern does not appear in the breath image inspection after the metal thin film on the glass substrate for photomask having a pattern formed on at least one surface with a metal thin film is dissolved and removed with an etching solution.
  • a regeneration processing step of forming a recycled glass substrate for a photomask by a processing method comprising:
  • a dissolution removal step of dissolving and removing the metal thin film using an etchant from a photomask having a glass substrate and a metal thin film formed in a pattern on one surface of the glass substrate, and after the dissolution removal step A regeneration treatment step of forming a regenerated glass substrate for a photomask by performing a wet wettability homogenization treatment step of bringing an aqueous alkaline solution into contact with the surface of the glass substrate and performing wet wettability homogenization treatment;
  • An etching step of etching an exposed portion of the metal thin film on which the resist is formed A method of manufacturing a photomask, comprising:
  • the wettability homogenization treatment described in the claims and specification of the present invention is not a surface treatment step such as a physical polishing step or dry etching, but a treatment in which an aqueous chemical solution is brought into contact with the surface of the glass substrate, Preferably, it is performed in a treatment step in which the surface of the glass substrate is immersed in an aqueous chemical solution.
  • the breath image inspection described in the claims and specification of the present invention is an inspection method in which water vapor is attached to the surface of a glass substrate and the wettability of the surface is visually inspected or automatically recognized.
  • the breath image inspection will be described in detail when the embodiment of the present invention is described.
  • the metal thin film described in the claims and specification of the present invention refers to a film that functions as a light-shielding film, a translucent film, etc. in a photomask, and not only a single metal as a metal material, but also an alloy, a nitride of a metal element, It is a concept that includes oxides, nitride oxides, and other compounds containing metal elements.
  • A. Method for Regenerating Glass Substrate for Photomask Refer to (P1) to (P5) of FIG. 3 for the photomask manufacturing process used in the process of manufacturing a flat display panel before explaining the present embodiment in the present invention. I will explain.
  • a photomask blank of a two-layered chromium film 2 is formed on a synthetic quartz substrate by sputtering pure chromium that increases the optical density and subsequently forming chromium oxide for suppressing reflection on the surface.
  • a pellicle is mounted on the film surface as necessary.
  • the photomask created in the above-described process is used by being mounted on various exposure apparatuses for production of various flat display panels.
  • the substrate is cleaned and dried.
  • the wet-wettability homogenization treatment liquid is an aqueous solution containing alkali as a main component, and the subsequent cleaning and drying steps and a series of continuous apparatus configurations are efficient.
  • the device configuration is placed vertically in the case holding the glass substrate to be recycled, placed in the vertical direction to circulate the wettability homogenizing solution, rinsed with pure water, etc.
  • Horizontal transfer equipment that transports horizontally with a mold transfer method and single wafers, applies wettability uniform treatment liquid from the top with a nozzle, then rinses with pure water, and finally performs drying with air A configuration is also possible.
  • the size of the water droplets formed by the condensation of water vapor will change, and the light scattering state will change throughout, so that a slight difference in the surface condition can be detected visually. can do.
  • FIG. 5a is a photomask having a pattern formed of a chrome film.
  • a chrome film portion (2a) is formed in a frame shape on the outer periphery of the photomask substrate, and the chrome film is finely patterned inside the photomask substrate.
  • the image portion (3a) thus arranged is arranged in multiple impositions.
  • FIG. 5 b is an image obtained by confirming the glass substrate from which the chromium film has been etched away by the breath image method. Thus, the outer shape of the patterns (2b and 3b) can be visually confirmed.
  • the fact that the breath image is not visually confirmed means that the outer shape of the original trace of the pattern formed by the chromium film in a state where water vapor is condensed on the glass surface cannot be seen.
  • the pattern (2b and 3b) formed with the original chromium film is not visible as shown in FIG. 5c.
  • the original pattern mark is confirmed by visual inspection of the reflection, and when the photomask blank is patterned again, white defects as shown in FIG. 6e are likely to occur at the pixel edge portion of the pattern.
  • Preliminary experiment 1 The regenerated glass substrate from which the chromium film was removed was added with hydrofluoric acid aqueous solution as solution 1, potassium hydroxide aqueous solution as solution 2, and organic phosphate, carboxylate, amic acid and surfactant as potassium hydroxide as solution 3. Immersion evaluation with an aqueous solution was performed.
  • the contents of the evaluation were the inspection of the pattern marks by the breath image method and the glass etching amount on the surface of the regenerated glass substrate which had been immersed for a predetermined time, washed with water and dried.
  • the immersion liquid temperature was 25 degrees and the immersion time was 2 hours, 5 hours, and 10 hours.
  • Both the 5% aqueous solution and the 10% aqueous solution (solution 1) of hydrofluoric acid had a large glass etching amount, and pattern marks were confirmed by the breath image method.
  • the etching amount in which the glass substrate was immersed for 10 hours was about 15 ⁇ m at 5% concentration and about 40 ⁇ m at 10% concentration.
  • aqueous solution of potassium hydroxide solution 2
  • no trace of traces was confirmed by the breath image method, and the amount of glass etching was less than that of hydrofluoric acid treatment, but the concentration of potassium hydroxide was high
  • the etching amount increased.
  • the etching amount when the glass substrate was immersed for 10 hours was about 1 ⁇ m at 5% concentration, about 3 ⁇ m at 10% concentration, about 4 ⁇ m at 15% concentration, and about 12 ⁇ m at 30% concentration.
  • the etching amount is preferably as small as possible.
  • Preliminary experiment 3 Preliminary experiment 3 will be described with reference to FIG. Next, the chromium film was dissolved and removed with an etching solution, and the substrate on which the original pattern trace was confirmed by the breath image method was immersed in Solution 2 and Solution 3, respectively, as shown in FIG. The effect in the same substrate was confirmed.
  • Table 2 shows the results of measuring the contact angle after removing the chromium film by etching and after immersing it in Solution 2 and Solution 3.
  • the contact angle was measured by immersing the glass surface of the portion where the chromium film was formed and the portion where the chromium film was not formed after etching away the chromium film and in the solution 2 and the solution 3 respectively for the same portion. It was measured later.
  • Table 2 shows the results of the contact angle measurement described above.
  • the contact angle was measured with a flat panel contact angle meter FPD-MH20 manufactured by Kyowa Interface Science.
  • the contact angle of the original chrome part was 19.2 degrees to 19.9 degrees, and the original glass part was 16.3 degrees to 16.5 degrees.
  • the difference in contact angle between the original chrome part and the original glass part is about 3 degrees, and it is considered that the original pattern trace could be confirmed by the breath image method.
  • the contact angles after immersing in solution 2 and solution 3 are 17.2 degrees to 17.8 degrees as shown in Table 2, and the contact angles of the original chrome part and the original glass part are both in contact.
  • the angle difference was 1 degree or less. More specifically, the difference between the contact angle of the original chrome part and the contact angle of the original glass part was 1 degree or less in the substrate after being immersed in an aqueous solution of potassium hydroxide of each concentration in the solution 2. . Moreover, also in the said board
  • a photosensitive material was applied to the chromium film-forming substrate, and a pattern was formed again by photolithography.
  • Fig. 6d shows the inspection result of the photomask on which the pattern was formed.
  • the inspection device used was a laser tech visual inspection device 51MD.
  • a detailed analysis of the location of the white defect shows the shape of the white defect at a location that intersects the original pattern trace, as shown in FIG. 6e. It was.
  • the glass substrate of the original pattern trace confirmed by the breath image method can be disappeared in a state that cannot be confirmed by the breath image method only by wet processing without depending on physical polishing. Further, it was confirmed that the pattern defect can be improved by erasing the original pattern trace by the breath image method.
  • a method for producing a reclaimed glass substrate for photomasks of the present invention includes a glass substrate and one of the glass substrates. Dissolving and removing the metal thin film by using an etchant from a photomask having a metal thin film formed in a pattern on the surface, and contacting the surface of the glass substrate after the dissolving and removing step with an alkaline aqueous solution And a wet wettability homogenization treatment step for performing wet wettability homogenization treatment.
  • the wettability of the surface of the recycled glass substrate can be uniformed. Therefore, when manufacturing a photomask using the recycled glass substrate, The metal thin film can be satisfactorily formed in a pattern on the surface of the recycled glass substrate, and peeling of the metal thin film can be prevented.
  • untreated glass when the photomask is manufactured again using the glass substrate after the dissolution and removal step (hereinafter may be referred to as an untreated glass substrate), untreated glass is used. There is a problem that the metal thin film formed on the substrate is easily peeled off and pattern defects are likely to occur.
  • a method of making the surface state uniform by polishing the surface of the untreated glass substrate is used, but there is a problem that the manufacturing cost is high. .
  • the present inventors have revealed that the untreated glass substrate was exposed to a glass substrate when used as a photomask.
  • the present invention has a great feature in finding the above points.
  • Dissolving and removing step dissolves and removes the metal thin film using an etchant from a photomask having a glass substrate and a metal thin film formed in a pattern on one surface of the glass substrate. It is a process. This step is a step of obtaining an untreated glass substrate.
  • the photomask has a glass substrate and a metal thin film formed in a pattern on the glass substrate.
  • the photomask used is one that has been used after the manufacture of a product using a photolithography process or one that has become defective during the manufacture of the photomask itself.
  • the glass substrate can be the same as that used for a general photomask, and examples thereof include synthetic quartz glass and Pyrex (registered trademark) glass. Moreover, about the thickness of a glass substrate, it selects suitably according to the use of a photomask, and it does not specifically limit.
  • the metal thin film used for the photomask can be the same as that used for a general photomask.
  • chromium (Cr), tantalum (Ta), molybdenum (Mo), titanium (Ti), zirconium A thin film mainly containing any one of metal elements selected from (Zr) or the like, or a thin film mainly containing any one of the nitride, oxide, or oxynitride of the metal element, or molybdenum silicide. (MoSi) thin film etc. are mentioned.
  • a metal thin film is comprised with chromium system materials, such as chromium, chromium nitride, chromium oxide, chromium oxynitride.
  • the thickness of the metal thin film can be appropriately selected according to the use of the photomask, and is, for example, about 30 nm to 150 nm.
  • the metal thin film in the photomask is usually formed on the surface of the glass substrate in a predetermined pattern.
  • a metal thin film it can select suitably according to the use etc. of a photomask.
  • the etching solution used in this step can be appropriately selected according to the type of metal thin film.
  • an etchant a general one can be used.
  • the metal thin film is made of a chromium-based material
  • the etching solution described in the section can be used.
  • the method etc. which immerse the metal thin film side surface of a photomask in etching liquid can be mentioned, for example.
  • the wet wettability homogenization treatment step in the present invention is a step of performing wet wettability homogenization treatment by bringing an alkaline aqueous solution into contact with the surface of the glass substrate after the dissolution and removal step.
  • a glass substrate that has been subjected to wet wettability homogenization treatment is referred to as a “treated glass substrate”, and a glass substrate in which the wettability of the glass substrate surface is uniform is referred to as a “recycled glass substrate”. May be explained.
  • the alkaline aqueous solution used in this step for example, a solution containing potassium hydroxide (KOH) as an alkaline component can be suitably used.
  • KOH potassium hydroxide
  • the concentration (content) of potassium hydroxide in the alkaline aqueous solution is not particularly limited as long as the wettability of the surface of the recycled glass substrate can be made uniform. It is preferably in the range of 30%, particularly in the range of 5% to 15%.
  • the concentration of potassium hydroxide is within the above-described range, the wettability of the surface of the glass substrate can be suitably made uniform.
  • an organic phosphate, a carboxylate, an amino acid, a surfactant, or the like may be added to the alkaline aqueous solution used in this step.
  • a method of bringing the alkaline aqueous solution into contact with the surface of the untreated glass substrate for example, a method of immersing the untreated glass substrate in an alkaline aqueous solution, or using a nozzle, a spray or the like on the surface of the untreated glass substrate on the metal thin film removal side
  • a method of spraying an alkaline aqueous solution or the like can be used.
  • FIGS. 7A and 7B are explanatory diagrams for explaining an example of the breath image inspection method used in the present invention.
  • a container 10 is prepared in which a treated glass substrate 1 ′ can be placed flat in an environment of normal temperature and normal humidity (23 ° C., humidity 50%).
  • the treated glass substrate 1 ′ is placed flat so that the surface that has been subjected to the wettability homogenization treatment (hereinafter, may be referred to as a treatment surface X) and the bottom surface of the container 10 face each other. .
  • a treatment surface X the surface that has been subjected to the wettability homogenization treatment
  • FIG. 7 (b) pure water 20 at about 80 ° C. is poured from the bottom of the container 10 to a height of about 1 cm to 2 cm, and left to stand for 1 minute, so that the water vapor 21 is treated with the treated glass. It adheres to the processing surface X of the substrate 1 ′.
  • the water vapor 21 attached to the processing surface X of the processed glass substrate 1 ′ is observed under a fluorescent lamp from the upper side of the container 10 through the surface Y opposite to the processing surface X of the processed glass substrate 1 ′.
  • a fluorescent lamp from the upper side of the container 10 through the surface Y opposite to the processing surface X of the processed glass substrate 1 ′.
  • the breath image inspection described above may be performed on the untreated glass substrate before the wettability homogenization treatment.
  • the wettability homogenization process and the breath image inspection are usually alternately performed until the wettability of the surface of the treated glass substrate is uniformized.
  • this process can be performed as follows, for example. First, an alkaline aqueous solution is brought into contact with the surface of an untreated glass substrate under various conditions to set optimum conditions for wet wettability homogenization treatment. In examining the optimum conditions, the wettability of the surface of the treated glass substrate is usually determined by the breath image inspection method described above. Next, in the production line, wet wettability homogenization treatment is performed on the plurality of untreated glass substrates under the optimum conditions described above.
  • FIG. 8 is an explanatory view for explaining another example of the breath image inspection method used in the present invention.
  • the treated glass substrate 1 ′ is fixed by the fixing device 50 or the like, and the treated surface X of the treated glass substrate 1 ′ is 80 ° C. using the steamer 30 or the like.
  • the pure water vapor 21 is attached.
  • the treated surface X of the treated glass substrate 1 ′ is observed by irradiating light 41 using the projector 40.
  • a general projector can be used.
  • the steamer as long as water vapor can be attached to the treated surface of the treated glass, the form and the like are not particularly limited, and a general one can be used. Examples of the steamer include hand steamer SSH-601 manufactured by Ishizaki Electric Co., Ltd.
  • the recycled glass substrate is usually subjected to washing and drying treatment.
  • the apparatus configuration (apparatus) described in the above-mentioned section “A. Recycling Method for Photomask Glass Substrate” can be preferably used.
  • the method for producing a recycled glass substrate for a photomask of the present invention is not particularly limited as long as it has the dissolution removal step and the wet wettability homogenization treatment step, and performs other steps as necessary. be able to.
  • the recycled glass substrate for a photomask of the present invention is used as a glass substrate for a photomask.
  • the photomask manufacturing method of the present invention has two aspects. Each will be described below.
  • the 1st aspect of the manufacturing method of the photomask of this invention is a breath image after melt
  • a regeneration processing step of forming a recycled glass substrate for photomask by a regeneration processing method that performs wet wettability homogenization processing until the pattern does not appear in inspection, and a metal thin film on at least one surface of the recycled glass substrate for photomask Forming a mask blank to form a mask blank, forming a resist on the metal thin film in a pattern, and etching an etching of the exposed portion of the metal thin film on which the resist is formed;
  • the manufacturing method characterized by having.
  • the regeneration processing step used in this aspect is a breath image inspection after dissolving and removing the metal thin film of the glass substrate for photomask having a pattern formed of a metal thin film on at least one surface with an etching solution.
  • a recycled glass substrate for a photomask is formed by a regeneration processing method in which wet wettability homogenization is performed until the pattern does not appear.
  • the regeneration processing method used in this embodiment can be the same as that described in the above-mentioned section “A. Recycling method of glass substrate for photomask”, and thus the description thereof is omitted here.
  • the mask blank formation process used for this mode is a process of forming a mask blank by forming a metal thin film on at least one side of the above-mentioned reproduction glass substrate for photomasks.
  • the material used for the metal thin film, the thickness of the metal thin film, and the like can be the same as those described in the above-mentioned section “B. Manufacturing method of recycled glass substrate for photomask”. Is omitted.
  • the method for forming a metal thin film can be the same as the method for forming a metal thin film used for a general photomask, and examples thereof include a vapor deposition method and a sputtering method.
  • the resist forming step used in this embodiment is a step of forming a resist in a pattern on the metal thin film.
  • a resist film is formed on a metal thin film, and the resist film is exposed and then developed to form a resist having a predetermined pattern shape.
  • the resist film is formed using a photosensitive resin.
  • the photosensitive resin used for the resist film can be the same as a general photosensitive resin, and may be a positive photosensitive resin or a negative photosensitive resin.
  • the positive photosensitive resin include phenol epoxy resin, acrylic resin, polyimide, and cycloolefin. Specific examples include IP3500 (manufactured by TOK), PFI27 (manufactured by Sumitomo Chemical), and ZEP7000 (manufactured by Zeon).
  • examples of the negative photosensitive resin include an acrylic resin. Specific examples include polyglycidyl methacrylate (PGMA), chemically amplified SAL601 (manufactured by Shipley Co., Ltd.), and the like.
  • the thickness of the resist film is not particularly limited, but is, for example, in the range of 10 nm to 10 ⁇ m. About the formation method of a resist film, it can be set as a well-known method.
  • the exposure method used in this step is not particularly limited as long as a desired pattern shape can be drawn on the resist film.
  • a laser drawing method, an EB drawing method, or the like can be used.
  • the exposure conditions and the like can be the same as those used at the time of manufacturing a general photomask, and thus description thereof is omitted here.
  • Examples of the method for developing the resist film include a method using a developer.
  • a general developer can be used as the type of the developer, but it is preferable to select appropriately according to the type of the photosensitive resin.
  • Specific examples of the developer include alkali developers such as tetramethylammonium aqueous solution, potassium hydroxide aqueous solution, sodium hydroxide aqueous solution and sodium carbonate aqueous solution, and acids such as hydrochloric acid aqueous solution, acetic acid aqueous solution, sulfuric acid aqueous solution and phosphoric acid aqueous solution.
  • a developing solution etc. can be mentioned.
  • the etching step used in this embodiment is a step of etching the exposed portion of the metal thin film on which the resist is formed.
  • a wet etching method or a dry etching method can be applied. In this step, it is particularly preferable to use a wet etching method. This is because it is advantageous in terms of cost.
  • a wet etchant obtained by adding perchloric acid to ceric ammonium nitrate can be preferably used.
  • resist stripping and photomask cleaning are performed.
  • the photomask manufacturing method of this embodiment is not particularly limited as long as it has the above-described regeneration processing step, resist formation step, and etching step, and the necessary steps can be appropriately selected and added. it can.
  • the photomask manufactured by the method for manufacturing a photomask according to this aspect can be used in a photolithography process when manufacturing various flat panels, circuit boards and the like.
  • 2nd aspect 2nd aspect of the manufacturing method of the photomask of this invention is the above-mentioned using etching liquid from the photomask which has the metal thin film formed in pattern shape on one surface of the glass substrate and the said glass substrate.
  • a regeneration processing step for forming a regenerated glass substrate for a mask a mask blank forming step for forming a mask blank by forming a metal thin film on at least one surface of the regenerated glass substrate for a photomask, and a resist on the metal thin film Resist forming process to form a pattern and etching the exposed part of the metal thin film on which the resist is formed And an etching process.
  • the steps other than the regeneration processing step and other matters can be the same as the contents described in the above-mentioned section “1. First embodiment”, and thus the description thereof is omitted here.
  • the regeneration processing step in this aspect can be the same as the content described in the above-mentioned section “B. Manufacturing method of recycled glass substrate for photomask”, and thus the description thereof is omitted here.
  • the present invention is not limited to the above embodiment.
  • the above-described embodiment is an exemplification, and the present invention has any configuration that has substantially the same configuration as the technical idea described in the claims of the present invention and exhibits the same function and effect. Are included in the technical scope.
  • Example 1 In the following, examples of the present invention were applied to a liquid crystal panel, and a reproduction process of a photomask of a synthetic quartz glass having a used glass substrate size of 450 mm ⁇ 550 mm and a thickness of 5 mm was performed.
  • the used photomask was made into a bare glass state by removing all of the chromium film with a chromium etching solution and performing pure water cleaning. As a result of the breath image inspection in this state, the original trace of the removed pattern was confirmed.
  • the recycled substrate from which the chromium film had been removed was immersed in a 5% aqueous KOH solution having a liquid temperature of 25 ° C. for 4 hours to perform pure water cleaning.
  • the glass etching amount was 0.6 ⁇ m.
  • a chromium blank substrate for a photomask was used in which a pure chromium film was formed on the main surface of the recycled glass substrate using a vacuum sputtering film forming apparatus and then a chromium oxide film was formed.
  • a chromium blank substrate for a photomask was used in which a pure chromium film was formed on the main surface of the recycled glass substrate using a vacuum sputtering film forming apparatus and then a chromium oxide film was formed.
  • the original pattern could not be confirmed.
  • Example 2 A reproduction process of a photomask created by the same method as in Example 1 was performed.
  • the photomask has been used, and reprocessing was performed to reuse the photomask substrate.
  • the used photomask was made into a bare glass state by removing all of the chromium film with a chromium etching solution and performing pure water cleaning. As a result of the breath image inspection in this state, the original trace of the removed pattern was confirmed.
  • the recycled substrate from which the chromium film was removed was immersed in a 10% aqueous solution of KOH having a liquid temperature of 25 ° C. for 4 hours to perform pure water cleaning.
  • the glass etching amount was 1.5 ⁇ m.
  • a chromium blank substrate for a photomask was used in which a pure chromium film was formed on the main surface of the recycled glass substrate using a vacuum sputtering film forming apparatus and then a chromium oxide film was formed.
  • the original pattern could not be confirmed.
  • a photomask having no dimensional abnormality and white defects peculiar to the reproduction substrate was obtained.
  • Example 3 A reproduction process of a photomask created by the same method as in Example 1 was performed.
  • the photomask has been used, and reprocessing was performed to reuse the photomask substrate.
  • the used photomask was made into a bare glass state by removing all of the chromium film with a chromium etching solution and performing pure water cleaning. As a result of the breath image inspection in this state, the original trace of the removed pattern was confirmed.
  • the recycled substrate from which the chromium film had been removed was immersed in Solution 3 having a liquid temperature of 25 ° C. for 4 hours and washed with pure water.
  • the glass etching amount was 1 ⁇ m or less, and as a result of the breath image inspection of the cleaned substrate, the original pattern disappeared, and a glass substrate for a photomask that could not be confirmed by visual inspection was obtained.
  • a chromium blank substrate for a photomask was used in which a pure chromium film was formed on the main surface of the recycled glass substrate using a vacuum sputtering film forming apparatus and then a chromium oxide film was formed.
  • a chromium blank substrate for a photomask was used in which a pure chromium film was formed on the main surface of the recycled glass substrate using a vacuum sputtering film forming apparatus and then a chromium oxide film was formed.
  • the original pattern could not be confirmed.
  • Example 2 In the same manner as in Example 1, all the chromium film was removed with a chromium etching solution, and pure water cleaning was performed to obtain a bare glass state. As a result of the breath image inspection of the recycled glass substrate in this state, the removed original pattern trace was confirmed.
  • a chromium blank substrate for a photomask was used in which a pure chromium film was formed on the main surface of the recycled glass substrate using a vacuum sputtering film forming apparatus and then a chromium oxide film was formed. As a result of visual inspection of the surface of the chrome blank substrate, the original pattern was confirmed.

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PCT/JP2013/075314 2012-09-26 2013-09-19 ガラス再生処理方法および再生ガラス基板とそれを用いたフォトマスクブランクスとフォトマスク WO2014050700A1 (ja)

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KR1020177031593A KR101963996B1 (ko) 2012-09-26 2013-09-19 유리 재생 처리 방법 및 재생 유리 기판과 그것을 사용한 포토마스크 블랭크와 포토마스크
JP2014538440A JP6256344B2 (ja) 2012-09-26 2013-09-19 ガラス基板の再生処理方法、再生ガラス基板の製造方法及びフォトマスクの製造方法
KR1020187034398A KR102085058B1 (ko) 2012-09-26 2013-09-19 유리 재생 처리 방법 및 재생 유리 기판과 그것을 사용한 포토마스크 블랭크와 포토마스크
KR1020157005441A KR101848983B1 (ko) 2012-09-26 2013-09-19 유리 재생 처리 방법 및 재생 유리 기판과 그것을 사용한 포토마스크 블랭크와 포토마스크
CN201380047359.8A CN104620176B (zh) 2012-09-26 2013-09-19 玻璃再生处理方法、再生玻璃基板及使用其的光掩模坯料和光掩模

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CN112404100A (zh) * 2020-11-03 2021-02-26 福建晶安光电有限公司 一种滤波器基片的回收工艺

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KR101963996B1 (ko) 2019-03-29
CN104620176A (zh) 2015-05-13
KR101848983B1 (ko) 2018-04-13
CN104620176B (zh) 2019-02-26
KR20170125119A (ko) 2017-11-13
KR102085058B1 (ko) 2020-03-05
CN109298594B (zh) 2021-12-24
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TW201427918A (zh) 2014-07-16
TWI558677B (zh) 2016-11-21
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