WO2017030109A1 - ペリクルフレーム、これを含むペリクル、ペリクルフレームの製造方法、およびペリクルの製造方法 - Google Patents
ペリクルフレーム、これを含むペリクル、ペリクルフレームの製造方法、およびペリクルの製造方法 Download PDFInfo
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- WO2017030109A1 WO2017030109A1 PCT/JP2016/073828 JP2016073828W WO2017030109A1 WO 2017030109 A1 WO2017030109 A1 WO 2017030109A1 JP 2016073828 W JP2016073828 W JP 2016073828W WO 2017030109 A1 WO2017030109 A1 WO 2017030109A1
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- WIPO (PCT)
- Prior art keywords
- pellicle
- frame
- film
- polyimide resin
- electrodeposition coating
- Prior art date
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- 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
- G03F1/62—Pellicles, e.g. pellicle assemblies, e.g. having membrane on support frame; Preparation thereof
- G03F1/64—Pellicles, e.g. pellicle assemblies, e.g. having membrane on support frame; Preparation thereof characterised by the frames, e.g. structure or material, including bonding means therefor
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- 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
- G03F1/62—Pellicles, e.g. pellicle assemblies, e.g. having membrane on support frame; Preparation thereof
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- 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
- G03F1/66—Containers specially adapted for masks, mask blanks or pellicles; Preparation thereof
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B15/00—Layered products comprising a layer of metal
- B32B15/04—Layered products comprising a layer of metal comprising metal as the main or only constituent of a layer, which is next to another layer of the same or of a different material
- B32B15/08—Layered products comprising a layer of metal comprising metal as the main or only constituent of a layer, which is next to another layer of the same or of a different material of synthetic resin
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B2311/00—Metals, their alloys or their compounds
- B32B2311/24—Aluminium
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B2379/00—Other polymers having nitrogen, with or without oxygen or carbon only, in the main chain
- B32B2379/08—Polyimides
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D11/00—Electrolytic coating by surface reaction, i.e. forming conversion layers
- C25D11/02—Anodisation
- C25D11/04—Anodisation of aluminium or alloys based thereon
- C25D11/18—After-treatment, e.g. pore-sealing
- C25D11/20—Electrolytic after-treatment
- C25D11/22—Electrolytic after-treatment for colouring layers
Definitions
- the present invention relates to a pellicle frame, a pellicle including the pellicle frame, a pellicle frame manufacturing method, and a pellicle manufacturing method.
- the pellicle is generally composed of a pellicle film that can transmit patterning light and a pellicle frame that supports the outer periphery of the pellicle film.
- the pellicle frame is made of a metal such as an aluminum alloy and may be anodized for surface protection.
- various ions such as sulfate ions are likely to remain in the anodized pellicle frame.
- the patterning accuracy is likely to decrease because residual ions are outgassing and the pellicle film is clouded, or the residual ions react with other ions to cause foreign substances.
- the electrodeposition coating film containing acrylic resin described in Patent Document 1 has low film strength. Therefore, there is a problem that the electrodeposition coating film is easily peeled off from the frame when the pellicle is attached to the exposure mask or when the pellicle is transported. In the manufacturing process of the pellicle frame, the surface of the pellicle frame may be rubbed, but it is assumed that the fluororesin film generates a lot of dust due to friction.
- the electrodeposition coating films of Patent Document 2 and Patent Document 3 have relatively high film strength.
- the patterning light is short-wavelength light (for example, excimer light such as KrF or ArF)
- the light is likely to be deteriorated by the light.
- the present invention has been made in view of such problems. That is, it is an object of the present invention to provide a pellicle frame that is not easily deteriorated by short-wavelength light such as excimer light and that is less likely to generate outgas and foreign matter, a pellicle using the pellicle frame, and a method of manufacturing the same. .
- a pellicle frame that supports the outer periphery of the pellicle film, and includes a frame and a film that includes a polyimide resin formed on a surface of the frame.
- the film containing the polyimide resin is an electrodeposition coating film.
- the electrodeposition coating film is a cured film of a composition containing a polycondensation polyimide resin, a thermally cross-linked imide resin, and a cationic polymer.
- the present invention also relates to the following pellicle frame manufacturing method and pellicle manufacturing method.
- the pellicle frame of the present invention or the pellicle using the pellicle frame, outgas is hardly generated from the pellicle frame, and further, foreign matter is hardly generated. Therefore, the patterning mask and pellicle film are not contaminated, and high-definition patterning is possible.
- FIG. 1 is a schematic sectional view showing an example of the structure of a pellicle according to the present invention.
- a numerical range expressed using “to” means a range including numerical values described before and after “to” as a lower limit value and an upper limit value.
- Pellicle frame The pellicle frame of the present invention has a frame and a film containing polyimide resin formed on the surface of the frame.
- anodized film is formed on the surface of the pellicle frame, ions adhering during the anodizing process elute and easily become foreign matter or outgas, which contaminates the mask or pellicle film. It was easy. Further, a film made of a fluororesin, an acrylic resin, an epoxy resin or the like has a problem that the film strength, heat resistance, abrasion resistance, light resistance and the like are not sufficient and are likely to deteriorate.
- the pellicle frame of the present invention has a film containing polyimide resin on the surface.
- Polyimide resin has very high resistance to light and heat, and is hardly decomposed by, for example, excimer light.
- membrane containing a polyimide resin has very high adhesiveness with metal frames. Therefore, when the pellicle frame is manufactured, when the pellicle and the exposure mask are bonded, or when the pellicle is transported, the film containing the polyimide resin is difficult to peel off from the frame. Furthermore, even if the frame is anodized, ion elution can be suppressed by the film containing the polyimide resin. Therefore, the pellicle having the pellicle frame is very useful as a protective member for various exposure masks.
- the presence or absence of dust adhering to the pellicle frame is inspected in a pellicle frame acceptance inspection process, a pellicle shipment inspection process in which a pellicle film is installed on the pellicle frame, and the like.
- the pellicle frame acceptance inspection step the pellicle frame is irradiated with strong light, and the presence or absence of dust is inspected by reflection of the light. If there is dust of an invisible size, the irradiated light will be reflected and shone. Therefore, only pellicle frames that do not reflect light are accepted.
- frame containing the polyimide resin of the pellicle frame of this invention are demonstrated.
- the shape of the frame of the pellicle frame of the present invention is appropriately selected according to the shape of the mask to be bonded to the pellicle.
- the material of the frame is not particularly limited as long as it can form a film containing a polyimide resin on the surface, and examples thereof include aluminum, aluminum alloy, magnesium alloy, titanium, brass, iron, stainless steel and the like.
- an aluminum alloy is preferable from the viewpoints of weight, workability, durability, and the like.
- a frame made of an aluminum alloy is also preferable from the viewpoint that a film containing a polyimide resin can be easily formed by electrodeposition coating.
- the frame may be surface-treated by plasma treatment, roughening treatment, sand blast treatment, shot blast treatment or the like. According to these treatments, foreign matters and oil components attached to the surface are removed. Therefore, when such a surface treatment is applied to the frame, the adhesion between the frame and the film containing the polyimide resin is likely to increase. Further, when the surface of the frame is roughened by the above processing, the surface of the pellicle frame is easily matted, and foreign matter attached to the surface of the pellicle frame is easily detected.
- the frame preferably has an anodized film formed by anodizing treatment from the viewpoint of the chemical stability of the pellicle frame.
- the method of anodizing the frame and its conditions are not particularly limited as long as the effects of the present invention are not impaired, and various conventionally known anodizing methods can be applied.
- a known anodizing method using sulfuric acid, phosphoric acid, nitric acid, tartaric acid or the like can be applied. Since the pellicle frame of the present invention has a film containing a polyimide resin to be described later on the surface of the frame, various ions are difficult to elute on the surface of the pellicle frame even if the frame is anodized.
- the anodized film is preferably an aluminum oxide film having a thickness of 5 ⁇ m or more and 70 ⁇ m or less and having pores having a diameter of 10 ⁇ m or more and 30 ⁇ m or less.
- the frame may be colored black (blackening treatment) after anodizing treatment by further electrolytic deposition treatment or the like.
- black black
- stray light is suppressed and dust is easily detected in the pellicle frame acceptance inspection that irradiates the pellicle frame with light and inspects for the presence of dust by light reflection.
- the type of metal deposited on the surface of the frame by electrolytic deposition is not particularly limited. For example, Ni (nickel), Co (cobalt), Cu (copper), Sn (tin), Mn (manganese), Fe ( Iron) and the like.
- the frame may be colored black by dyeing with a black dye.
- the frame can be dyed with a black dye by a known method. For example, a method is known in which an organic dye or the like is infiltrated into a film produced by anodizing to make it black.
- the frame is preferably not subjected to sealing treatment after anodizing treatment.
- sealing treatment aluminum hydroxide or the like is formed on the surface by the sealing treatment, the electrical conductivity on the surface of the frame is lowered, so that it is difficult to form a post-electrodeposition coating film.
- the film containing polyimide resin is a film formed on the surface of the frame.
- the thickness of the film containing the polyimide resin is preferably 0.5 ⁇ m or more and less than 30 ⁇ m, more preferably 5 ⁇ m or more and less than 30 ⁇ m, and further preferably 7 ⁇ m or more and 25 ⁇ m or less.
- the method for forming the film containing the polyimide resin is not particularly limited, and the polyimide coating can be formed on the surface of the frame by various coating methods. Specific coating methods include spray coating, electrodeposition coating, dip coating, and the like. Spray coating and electrodeposition coating are preferable. On the other hand, the polyimide coating is appropriately selected depending on the coating method.
- a film formed by spray coating also referred to as “spray coating film”
- a film formed by electrodeposition coating also referred to as “electrodeposition coating film”.
- Spray coating film is a film formed on the surface of a frame by a spray coating method, and includes a polyimide resin.
- a film containing a polyimide resin is formed by a spray coating method, after adjusting the concentration of polyimide or a precursor thereof with a diluent, the paint is sprayed together with high-pressure air from a spray nozzle of a spray coating apparatus. Then, the particles of the paint sprayed from the spray nozzle are uniformly attached to the above-described frame, and are cured by heating or the like as necessary.
- a general polyimide paint can be applied by spray coating.
- examples thereof include paints described in JP2009-221398, JP2009-091573, JP2007-332369, and the like.
- Electrodeposition coating film is a film formed on the surface of the frame by an electrodeposition coating method, and includes a polyimide resin.
- the electrodeposition coating film may be a film formed by a cationic electrodeposition coating method or a film formed by an anion electrodeposition coating method. From the viewpoint of obtaining a film having a good appearance, that is, a coating film having a flat surface state, a film formed by a cationic electrodeposition coating method is preferable.
- the electrodeposition coating film can be obtained by electrodeposition coating by a method described later using a composition for electrodeposition coating containing a polyimide resin, a precursor thereof, or a modified body thereof.
- a composition for electrodeposition coating containing a polyimide resin, a precursor thereof, or a modified body thereof containing a polyimide resin, a precursor thereof, or a modified body thereof.
- composition for cationic electrodeposition coating can be, for example, a composition containing (A) a polyimide resin, (B) a cationic polymer, (C) a neutralizing agent, and (D) an aqueous medium. Further, instead of (A) the polyimide resin and (B) the cationic polymer, (A ′) a cation-modified polyimide resin in which the polyimide resin is cation-modified may be included. Moreover, the composition for cationic electrodeposition coating may contain (E) a pigment and (F) other components as needed. Hereinafter, these components will be described.
- the polyimide resin contained in the composition for cationic electrodeposition coating is not particularly limited.
- the polyimide resin preferably includes, for example, a “polycondensation polyimide resin” having a repeating unit represented by the following general formula (1) from the viewpoint of increasing the heat resistance and light resistance of the electrodeposition coating film.
- the “polycondensation polyimide resin” as used in the present invention refers to a polyimide resin obtained by polycondensation of tetracarboxylic dianhydride and diamine, and is a wholly aromatic polyimide, wholly aliphatic polyimide, semi-aromatic. Any of the group (semi-aliphatic) polyimides may be used. However, polycondensation polyimide resin does not include “thermally crosslinked imide resin” described later.
- a in the general formula (1) is selected from divalent groups represented by the following general formula.
- Z 1 to Z 10 in the above general formula are respectively a phenylenediamine residue, a naphthalenediamine residue, an anthracenediamine residue, a phenanthrenediamine residue, an alkanediamine residue in which x in the general formula C x H 2x is 6 to 12,
- X 1 to X 6 are each a single bond, —O—, —S—, —CO—, —COO—, —C (CH 3 ) 2 —, —C (CF 3 ) 2 —, —SO 2 — or —NHCO—.
- Z 1 to Z 10 and X 1 to X 6 contained in a plurality of A may be the same or different.
- the divalent group containing an aromatic ring that may be A in the general formula (1) may be a divalent group derived from an aromatic diamine.
- aromatic diamines include m-phenylenediamine, o-phenylenediamine, p-phenylenediamine, 1,4-diaminonaphthalene, 1,5-diaminonaphthalene, 1,8-diaminonaphthalene, 2,6-diaminonaphthalene.
- aromatic diamines examples include m-phenylenediamine, o-phenylenediamine, p-phenylenediamine, 3,3′-diaminodiphenyl ether, 3,4′-diaminodiphenyl ether, 4,4′-diaminodiphenyl ether, 3, 3'-diaminodiphenylsulfone, 4,4'-diaminodiphenylsulfone, 3,3'-diaminobenzophenone, 3,3'-diaminodiphenylmethane, 4,4'-diaminodiphenylmethane, 1,3-bis (3-aminophenoxy ), Benzene, 1,3-bis (4-aminophenoxy) benzene, and 4,4′-bis (3-aminophenoxy) biphenyl are more preferable, and m-phenylenediamine, o-phenylenediamine, and p-phenyl
- alkenyl group that can be A in the general formula (1) or the divalent group containing an alicyclic structure can be an aliphatic diamine or a divalent group derived from an alicyclic diamine.
- preferred aliphatic diamines and alicyclic diamines include 1,5-diaminopentane, 1,6-diaminohexane, cyclobutanediamine, cyclohexanediamine, bis (aminomethyl) cyclohexane, diaminobicycloheptane, norbornane diamine, diaminomethyl.
- Bicycloheptane diaminooxybicycloheptane, oxanorbornanediamine, diaminomethyloxybicycloheptane, isophoronediamine, diaminotricyclodecane, diaminomethyltricyclodecane, bis (aminocyclohexyl) methane, bis (aminocyclohexyl) isopropylidene, etc. included.
- More preferred aliphatic diamines include cyclohexanediamine, 1,4-bis (aminomethyl) cyclohexane, and diaminomethylbicycloheptane.
- the polyimide resin in the present invention only one kind of the diamine may be contained or plural kinds thereof may be contained. Moreover, either one of aromatic diamine and aliphatic diamine may be contained, and both may be contained.
- B in the general formula (1) is selected from tetravalent groups represented by the following formula.
- W 1 to W 10 in the above formula are tetravalent groups containing an aromatic ring such as benzene, naphthalene, anthracene, phenanthrene and perylene; cyclobutane, cyclopentane, cyclohexane, cyclodecane, bicycloheptanes, bicyclooctanes, tetrahydrofurans, etc.
- a tetravalent group containing the following alicyclic structure: Y 1 to Y 5 are each a single bond, —O—, —S—, —CO—, —COO—, —C (CH 3 ) 2 —, —C (CF 3 ) 2 —, —SO 2. -Or -NHCO-.
- W 1 to W 10 and Y 1 to Y 5 included in the plurality of B may be the same or different.
- the tetravalent group containing an aromatic ring that may be B in the general formula (1) may be a tetravalent group derived from a tetracarboxylic dianhydride containing an aromatic ring.
- tetracarboxylic dianhydrides containing aromatic rings include pyromellitic dianhydride, 3,3 ′, 4,4′-biphenyltetracarboxylic dianhydride, 2,3,3 ′, 4-biphenyl -Tetracarboxylic dianhydride, 3,3 ', 4,4'-benzophenone tetracarboxylic dianhydride, 3,3', 4,4'-diphenylsulfone tetracarboxylic dianhydride, 4,4'- Oxydiphthalic dianhydride, 1,2,4,5-naphthalenetetracarboxylic dianhydride, 1,2,5,6-naphthalenetetracarboxylic dianhydride, 1,2,6,7-
- the tetravalent group containing an alicyclic structure may be a tetravalent group derived from a tetracarboxylic dianhydride containing an alicyclic structure.
- Preferred examples of the tetracarboxylic dianhydride containing an alicyclic structure include cyclobutane tetracarboxylic dianhydride, 1,2,3,4-cyclopentanetetracarboxylic dianhydride, 1,2,4,5 Cyclohexanetetracarboxylic dianhydride, bicyclo [2.2.1] heptane-2,3,5,6-tetracarboxylic dianhydride, bicyclo [2.2.2] oct-7-ene-2, 3,5,6-tetracarboxylic dianhydride, bicyclo [2.2.2] octane-2,3,5,6-tetracarboxylic dianhydride, 2,3,5-tricarboxycyclopentylace
- Examples of preferred tetracarboxylic dianhydrides include pyromellitic dianhydride, 3,3 ′, 4,4′-biphenyltetracarboxylic dianhydride, 2,3,3 ′, 4-biphenyl-tetracarboxylic Acid dianhydride, 3,3 ′, 4,4′-benzophenone tetracarboxylic dianhydride, 4,4′-oxydiphthalic dianhydride, 3,3 ′, 4,4′-diphenylsulfone tetracarboxylic acid dianhydride Anhydride, 2,2-bis [(3,4-dicarboxyphenoxy) phenyl] propane dianhydride, 2,2-bis (3,4-dicarboxyphenyl) -1,1,1,3,3 3-hexafluoropropane dianhydride, cyclobutanetetracarboxylic dianhydride, 1,2,4,5-cyclohexanetetracarboxylic dianhydride.
- pyromellitic dianhydride 3,3 ′, 4,4′-biphenyltetracarboxylic dianhydride, 2,2-bis [(3,4-dicarboxyphenoxy) phenyl] propane dianhydride 2,2-bis (3,4-dicarboxyphenyl) -1,1,1,3,3,3-hexafluoropropane dianhydride, cyclobutanetetracarboxylic dianhydride, 1,2,4,5 -Cyclohexanetetracarboxylic dianhydride.
- the polyimide resin in the present invention may contain only one kind of the acid dianhydride or plural kinds. Moreover, either one of aromatic acid dianhydride and aliphatic acid dianhydride may be contained, and both may be contained.
- the polycondensation polyimide resin is preferably contained in the composition for cationic electrodeposition coating in an amount of 5 to 50% by mass, more preferably 10 to 40% by mass.
- amount of the polycondensation polyimide resin is within the above range, (D) dispersibility in an aqueous medium is likely to increase.
- the polyimide resin preferably contains a “thermally crosslinked imide resin” together with the “polycondensation polyimide resin”.
- the “thermally crosslinked imide resin” in the present invention refers to a resin containing an imide bond and a thermally crosslinkable group such as an unsaturated double bond at the molecular end.
- the thermally cross-linked imide resin is easily compatible with the above-mentioned polycondensation polyimide resin and the (B) cationic polymer described later.
- the composition for cationic electrodeposition coating contains a thermally cross-linked imide resin
- the dispersibility of the polycondensation polyimide resin in an aqueous medium increases, or the precipitation of the polycondensation polyimide resin increases during cationic electrodeposition coating.
- the thermally cross-linked imide resin reacts with each other, or the cross-linkable group of the heat cross-linked imide resin reacts with the OH group of the cationic polymer (B) described later to form a cross-linked structure.
- the composition for cationic electrodeposition coating contains a thermally cross-linked imide resin, the film strength of the obtained electrodeposition coating film tends to increase.
- thermally cross-linked imide resins examples include N, N′-m-xylene bismaleimide, N, N′-4,4′-diphenylmethane bismaleimide, 2,2-bis [4- (4-maleimidophenoxy) phenyl] Propane, N, N'-m-phenylene bismaleimide, N, N'-4,4'-diphenyl ether bismaleimide, N, N'-m-xylene bisnadiimide, N, N'-4,4'-diphenylmethane bis Allyl nadiimide and the like are included.
- the thermally cross-linked imide resin is preferably contained in the cationic electrodeposition coating composition in an amount of 10 to 80% by mass, more preferably 15 to 60% by mass, and further preferably 20 to 50% by mass.
- amount of the thermally cross-linked imide resin is within the above range, (D) the dispersibility of the polycondensation polyimide resin or the like in the aqueous medium is likely to increase, and the strength of the electrodeposition coating film is likely to increase.
- the cationic polymer may be a polymer containing at least one cationic group such as an amino group or a quaternized salt of an amino group.
- the composition for cationic electrodeposition coating includes (B) a cationic polymer, the (B) cationic polymer and the (A) polyimide resin can be used without introducing a cationic group directly into the above-described (A) polyimide resin. Due to the compatibility or the like, (A) the polyimide resin can be deposited on the surface of the frame.
- the cationic polymer can be, for example, an acrylic copolymer or an epoxyamine adduct resin.
- acrylic copolymer examples include a copolymer obtained by copolymerizing an amino derivative of (meth) acrylic acid, a hydroxy derivative of (meth) acrylic acid, and a vinyl ester.
- (meth) acryl means either one or both of acrylic and methacrylic.
- amino derivatives of (meth) acrylic acid examples include dimethylaminoethyl (meth) acrylate, diethylaminoethyl (meth) acrylate, ethyltrimethylammonium chloride (meth) acrylate, and the like.
- examples of hydroxy derivatives of (meth) acrylic acid include 2-hydroxyethyl (meth) acrylate, 3-hydroxypropyl (meth) acrylate, 4-hydroxybutyl (meth) acrylate, and (meth) acrylic acid. 2-hydroxy-3-phenoxypropyl and the like are included.
- vinyl esters include methyl (meth) acrylate, 2-ethylhexyl (meth) acrylate, n-butyl (meth) acrylate, isobutyl (meth) acrylate, benzyl (meth) acrylate, (meth ) Cyclohexyl acrylate, isobornyl acrylate, 2- (perfluorooctyl) ethyl methacrylate, trifluoromethyl methacrylate and the like.
- the epoxyamine adduct resin may be a derivative obtained by modifying the epoxy group of the epoxy resin with a primary amine or a secondary amine.
- epoxy resins include bisphenol A type epoxy resins (trade names: jER resins 828, 834, 1001, 1004, 1007, 1009 (manufactured by Mitsubishi Chemical Corporation)); novolac phenol type epoxy resins (trade names: jER resin 152, 154 (manufactured by Mitsubishi Chemical Corporation)) and the like.
- Examples of the primary amine for modifying the epoxy resin include monomethanolamine, monoethanolamine, mono-n-propanolamine, monoisopropanolamine, dimethylaminoethylamine, diethylaminoethylamine, diethylaminopropylamine and the like.
- Examples of secondary amines include dimethanolamine, diethanolamine, di-n-propanolamine, diisopropanolamine, methylethanolamine, methylpropanolamine, di-n-butylamine and the like.
- the cationic polymer is preferably contained in the cationic electrodeposition coating composition in an amount of 10 to 70% by mass, more preferably 20 to 70% by mass, and further preferably 30 to 60% by mass.
- amount of the (B) cationic polymer is within the above range, (D) the dispersibility of the (A) polyimide resin in the aqueous medium is likely to increase.
- amount of the (B) cationic polymer is within the above range, the amount of the (A) polyimide resin is relatively sufficient, and thus the heat resistance and the like of the electrodeposition coating film are likely to be sufficiently increased.
- the cationic electrodeposition coating composition contains (A ′) a cation-modified polyimide resin instead of the aforementioned (A) polyimide resin and (B) cationic polymer. But you can.
- the composition for cationic electrodeposition coating contains (A ′) a cation-modified polyimide resin
- the composition for cationic electrodeposition coating needs to separately contain (B) a cationic polymer composed of the above-mentioned acrylic resin or epoxy resin. Absent. Therefore, the heat resistance of the electrodeposition coating film is more likely to increase.
- the cation-modified polyimide resin may be a resin in which a cationic group is bonded to the above-described (A) polyimide resin via a urea bond or a urethane bond.
- the cationic group include a primary amino group, a secondary amino group, and a tertiary amino group.
- a method for bonding a cationic group to the above-mentioned (A) polyimide resin there is the following method.
- examples of the “cationic-containing compound” include polyfunctional amines, hydroxyl group-containing amines, ketiminated amines, hydroxyl group-containing ketimines, and the like. These may be used alone or in combination of two or more.
- the polyfunctional amine may be a compound having two or more amino groups in one molecule. Examples thereof include N, N-dimethylethylenediamine, N, N-dimethylpropylenediamine, ethylenediamine, propylenediamine, and diethylenetriamine. Is included.
- hydroxyl group-containing amine examples include alkanolamines such as ethanolamine, propanolamine, isopropanolamine, N-methylethanolamine, N-methyldiethanolamine, N, N-dimethylethanolamine and the like.
- ketiminated amines examples include ketiminated amines obtained by reacting the above polyfunctional amines with ketones such as acetone, methyl ethyl ketone, and methyl isobutyl ketone.
- hydroxyl group-containing ketimines are obtained by reacting aminoalkylalkanolamines such as aminoethylethanolamine, aminoethylpropanolamine, aminoethylisopropanolamine, aminopropylethanolamine, aminopropylpropanolamine and the above ketones.
- aminoalkylalkanolamines such as aminoethylethanolamine, aminoethylpropanolamine, aminoethylisopropanolamine, aminopropylethanolamine, aminopropylpropanolamine and the above ketones.
- aminoalkylalkanolamines such as aminoethylethanolamine, aminoethylpropanolamine, aminoethylisopropanolamine, aminopropylethanolamine, aminopropylpropanolamine and the above ketones.
- aminoalkylalkanolamines such as aminoethylethanolamine, aminoethylpropanolamine, aminoethy
- the cation-modified polyimide resin is preferably contained in the cationic electrodeposition coating composition in an amount of 5 to 70% by mass, more preferably 10 to 60% by mass.
- amount of the (A ′) cation-modified polyimide resin is within the above range, the heat resistance of the electrodeposition coating film is likely to be sufficiently increased, and the electrodeposition coating film can be efficiently formed.
- the composition for cationic electrodeposition coating contains the neutralizing agent for improving the dispersibility to the aqueous medium of the above-mentioned (B) cationic polymer and (A ') cation modified polyimide resin.
- the neutralizing agent include hydrochloric acid, nitric acid, phosphoric acid, formic acid, acetic acid, lactic acid, succinic acid, inorganic acids such as butyric acid, and organic acids.
- the neutralizing agent is preferably contained so that the pH of the cationic electrodeposition coating composition is in the range of 3 to 5.
- the aqueous medium contained in the composition for cationic electrodeposition coating is ion-exchanged water, pure water or the like.
- the aqueous medium may contain a small amount of alcohol or the like as required.
- the amount of the aqueous medium (D) contained in the cationic coating composition is appropriately selected according to the viscosity and the like of the cationic coating composition.
- composition for cationic electrodeposition coating may contain a pigment such as carbon black.
- a pigment such as carbon black.
- the content of the pigment is generally 1 to 35% by mass, preferably 10 to 30% by mass, based on the total solid content of the composition for cationic electrodeposition coating.
- the cationic electrodeposition coating composition may contain other components as necessary.
- other components include water-miscible organic solvents, surfactants, antioxidants, ultraviolet absorbers and the like.
- composition for cationic electrodeposition coating may be a composition obtained by preparing each of the above components, but may be a commercially available composition for electrodeposition coating.
- commercially available compositions for cationic electrodeposition coating include Elecoat PI manufactured by Shimizu Corporation.
- the electrodeposition coating film comprises 1) a step of forming a film of the above-mentioned cationic electrodeposition coating composition on the surface of the frame, and 2) heat curing and drying the obtained film to obtain a cured electrodeposition coating film. And a process.
- a frame which is an object to be coated is immersed in an electrodeposition tank charged with the cationic electrodeposition coating composition.
- the frame is used as a cathode, and a voltage is applied between the anode and the above-described (A) polyimide resin and (B) cationic polymer or (A ′) cation-modified polyimide resin. Thereby, a film containing polyimide resin is formed on the frame surface.
- the electrodeposition coating is preferably performed at a voltage of 100 to 220 V and an energization time of 30 to 240 seconds.
- the thickness of the film (wet film) after electrodeposition coating is preferably 5 ⁇ m or more and less than 30 ⁇ m, and more preferably 7 ⁇ m or more and 25 ⁇ m or less.
- the film after electrodeposition coating is too thin, the cohesive force of the electrodeposition coating film obtained by curing the film is not sufficient, and it is difficult to obtain desired heat resistance and film strength.
- the thickness of the film after electrodeposition coating is too thick, the film surface may become rough and may become a cocoon skin-like surface, which is not only inferior in smoothness but also finally obtained in the electrodeposition coating film The thickness of the is difficult to be uniform.
- the thickness of the film after electrodeposition coating is adjusted according to the voltage and energization time during electrodeposition coating.
- step 2) Rinsing the membrane obtained in step 1) with water. Thereafter, in step 2), the pellicle frame is baked at 120 to 260 ° C., preferably 140 to 220 ° C. for 10 to 30 minutes to heat and cure the electrodeposition coating film to obtain an electrodeposition coating film.
- the thickness of the electrodeposition coating film (cured film) is almost the same as the above-mentioned film thickness, preferably 5 ⁇ m or more and less than 30 ⁇ m, more preferably 7 ⁇ m or more and 25 ⁇ m or less.
- the pellicle frame of the present invention can be manufactured by manufacturing a frame and forming a film containing a polyimide resin on the frame.
- the manufacturing method of the pellicle frame can be appropriately selected according to the type of frame, the method of forming a film having a polyimide resin, and the like.
- the step of anodizing the aluminum alloy frame, the step of blackening the surface of the aluminum alloy frame, and the blackened aluminum alloy frame includes a polyimide resin.
- a pellicle frame can be manufactured by applying a paint (spray coating or electrodeposition coating) to form a film containing a polyimide resin.
- the pellicle of the present invention includes a pellicle film, the pellicle frame that supports the outer periphery of the pellicle film, a film adhesive that bonds the pellicle frame and the pellicle film, and the pellicle frame and the mask. And a mask adhesive.
- FIG. 1 shows an example of a pellicle according to the present invention.
- the pellicle 10 includes a pellicle film 12 and a pellicle frame 14 that supports the outer periphery of the pellicle film 12.
- the pellicle film 12 is stretched through a film adhesive layer 13 on one end face of the pellicle frame 14.
- a mask adhesive layer 15 is provided on the other end surface of the pellicle frame 14.
- the pellicle film 12 is held by a pellicle frame 14 and covers an exposure area of a mask (not shown). Therefore, the pellicle film 12 is a film having translucency so as not to block energy (light) by exposure.
- the material of the pellicle film 12 include quartz glass, a transparent material such as a fluororesin and cellulose acetate.
- the film adhesive layer 13 bonds the pellicle frame 14 and the pellicle film 12 together.
- the mask adhesive layer 15 bonds the pellicle frame 14 and the mask (not shown).
- the film adhesive layer 13 can be, for example, a fluoropolymer such as an acrylic resin adhesive, an epoxy resin adhesive, a silicone resin adhesive, a fluorine-containing silicone adhesive, or a fluorine-containing ether adhesive.
- the mask adhesive layer 15 may be, for example, a double-sided adhesive tape, a silicone resin adhesive, an acrylic adhesive, a rubber adhesive, a vinyl adhesive, an epoxy adhesive, or the like.
- the pellicle 10 is mounted on a mask (not shown) via a mask adhesive layer 15 to prevent foreign matters from adhering to the mask (not shown).
- the foreign matter adhering to the mask causes poor resolution on the wafer when the exposure light is focused on it. Therefore, the pellicle 10 is mounted so as to cover an exposure area of a mask (not shown).
- the mask (not shown) is a glass substrate on which a patterned light-shielding film is arranged.
- the light shielding film is a single layer or multiple layer film of a metal such as Cr or MoSi.
- a mask including a patterned light-shielding film becomes an exposure area.
- Exposure light used for lithography such as a process for forming a circuit pattern drawn on a semiconductor element is a short wavelength such as a mercury lamp i-line (wavelength 365 nm), KrF excimer laser (wavelength 248 nm), ArF excimer laser (wavelength 193 nm), etc. Can be the light.
- the film containing the polyimide resin included in the pellicle frame of the present invention has excellent film strength while having good adhesion to the metal (frame). Further, ion elution from the frame can be suppressed by the film containing the polyimide resin. Therefore, dust generation due to peeling of the film containing the polyimide resin hardly occurs, and further generation of gas from the pellicle frame, generation of foreign matters, and the like hardly occur. Further, the film containing the polyimide resin is difficult to be decomposed by irradiation with excimer laser light (ArF light, KrF light, or the like). Therefore, the pellicle having the pellicle frame can be applied to various patterning.
- the pellicle can be produced by forming a layer made of a film adhesive on the pellicle frame and attaching a pellicle film on the film adhesive.
- Example 1 An aluminum frame (size: 149 mm ⁇ 122 mm ⁇ height 5.8 mm, support frame thickness 2 mm) made of JIS A7075-T6 was prepared. The frame was annealed in the atmosphere at a temperature of 250 ° C. for 20 minutes. Thereafter, the surface of the frame was shot blasted with stainless steel having an average diameter of about 100 ⁇ m. Next, the frame was anodized using an electrolytic bath of 15% by mass sulfuric acid at an electrolysis voltage of 20 V and an electric quantity of 10 C / cm 2 .
- an electrolytic deposition bath in which nickel sulfate hexahydrate 160 g / L, boric acid 40 g / L, tartaric acid 3 g / L, and magnesium oxide 1 g / L were dissolved was used for constant voltage electrolysis at 30 ° C. and AC voltage 15 V. Then, electrolytic deposition treatment was performed for 6 minutes. As a result, a colored frame was obtained. Then, the frame was washed with pure water, placed in a bathtub containing a cationic polyimide electrodeposition paint (Elecoat PI manufactured by Shimizu Corporation), and electrodeposition-coated at 25 ° C. and a voltage of 100 V for 1 minute.
- a cationic polyimide electrodeposition paint (Elecoat PI manufactured by Shimizu Corporation)
- the frame after electrodeposition coating is washed with water, dried at 100 ° C. for 15 minutes, and then baked at 180 ° C. for 30 minutes to form an electrodeposition coating film (a film containing polyimide resin) having a thickness of 10 ⁇ m on the frame.
- a pellicle frame 1 was obtained.
- Example 2 A pellicle frame 2 was produced in the same manner as in Example 1 except that the anodizing treatment and electrodeposition coating were performed under the following conditions.
- An alkaline aqueous solution in which 53 g / L of sodium tartrate dihydrate and 4 g / L of sodium hydroxide were dissolved was used as an electrolytic solution, and anodization was performed under the conditions of 5 ° C., electrolytic voltage 30 V, and electric quantity 10 C / cm 2 .
- Electrodeposition coating The frame after the electrolytic deposition treatment was washed with pure water and placed in a bathtub containing a cationic polyimide electrodeposition paint (Elecoat PI manufactured by Shimizu Corporation). A carbon plate was used for the anode and a frame was used for the cathode, and electrodeposition was applied at 25 ° C. and a voltage of 100 V for 1 minute. Thereafter, washing, drying and baking were performed in the same manner as in Example 1 to obtain an electrodeposition coating film (a film containing a polyimide resin) having a thickness of 9 ⁇ m.
- a cationic polyimide electrodeposition paint (Elecoat PI manufactured by Shimizu Corporation). A carbon plate was used for the anode and a frame was used for the cathode, and electrodeposition was applied at 25 ° C. and a voltage of 100 V for 1 minute. Thereafter, washing, drying and baking were performed in the same manner as in Example 1 to obtain an electrodeposition coating film (a film containing a polyimide resin) having
- Example 3 A frame material made of aluminum alloy 7075 having an outer dimension of 148.95 mm ⁇ 114.95 mm ⁇ thickness 2.50 mm having a frame shape was subjected to anodizing treatment under the following conditions. Thereafter, the same electrodeposition coating as in Example 2 was performed to produce a pellicle frame 3 on which an electrodeposition coating film (a film containing a polyimide resin) having a thickness of 5 to 20 ⁇ m was formed.
- an electrodeposition coating film a film containing a polyimide resin
- An alkaline aqueous solution in which an inorganic acid hydrate is dissolved is used as an electrolyte, a solution having a pH of 12 to 14, a bath temperature of 0 to 20 ° C., a voltage of 0.5 V to less than 20 V, and a treatment time of 2 to 120 minutes. Anodization was performed under the conditions.
- Example 4 The frame material made of aluminum alloy 7075 having an outer dimension of 148.95 mm ⁇ 114.95 mm ⁇ thickness 2.50 mm forming a frame shape was anodized in the same manner as in Example 3. Thereafter, an anionic polyimide electrodeposition paint manufactured by PI Engineering Laboratory Co., Ltd. was electrodeposited to produce a pellicle frame 4 on which an electrodeposition coating film (a film containing polyimide resin) having a thickness of 5 to 20 ⁇ m was formed. .
- the electrodeposition coating film (film containing polyimide resin) of the pellicle frame 4 was more coated than the electrodeposition coating film (film containing polyimide resin) of the pellicle frame 3. The condition was rough.
- Example 5 Similar to Example 3, the frame material was similarly subjected to anodizing treatment. Thereafter, a polyimide coating made by IST was diluted with a diluent solvent. Then, the paint was sprayed to produce a pellicle frame 5 on which a spray coating film (a film containing polyimide resin) having a thickness of 0.5 to 20 ⁇ m was formed.
- a spray coating film a film containing polyimide resin
- a pellicle frame 6 was produced in the same manner as in Example 1 except that the sealing treatment was performed under the following conditions.
- sealing treatment The frame after the electrolytic deposition treatment was placed in a vapor sealing device, and sealing treatment was performed for 30 minutes while generating water vapor at a relative humidity of 100%, 2.0 kg / cm 2 G, and 130 ° C.
- a pellicle frame 7 was produced in the same manner as in Example 2 except that the sealing treatment was performed under the following conditions instead of the electrodeposition coating. (Sealing treatment) The frame after the electrolytic deposition treatment was placed in a vapor sealing device, and sealing treatment was performed for 30 minutes while generating water vapor at a relative humidity of 100%, 2.0 kg / cm 2 G, and 130 ° C.
- the measurement sample in the drum-type quartz cell was irradiated with ArF laser for 5 minutes under the conditions of 1000 Hz and 0.4 mJ / cm 2 .
- a substance released as a gas from the measurement sample surface by ArF laser irradiation was collected in a collection tube to obtain a generated gas sample.
- the amount of a substance collected by a collection tube using a heat desorption gas chromatograph mass spectrometer (GC-MS) was measured as a generated gas amount (in undecane conversion).
- a thermal desorption GC-MS TDTS-2010
- GC-2010 gas chromatograph
- GCMS-QP2010 mass spectrometer manufactured by Shimadzu Corporation were used. The results are shown in Table 1.
- the electrodeposition coating film (film containing polyimide resin) of the pellicle frame of Example 1 and the spray coating film (film containing polyimide resin) of the pellicle frame of Example 5 are Comparative Example 1.
- the outgas amount was small. This is presumably because the films containing the polyimide resins of Examples 1 and 5 were difficult to be decomposed by ArF excimer laser light.
- the absorption coefficient of ArF laser light (wavelength: 193 nm) is about 0.15 ⁇ m ⁇ 1 for acrylic resins, and polyimide The resin is 20 ⁇ m ⁇ 1 . Therefore, as long as the absorbance is compared, it is presumed that the polyimide resin that easily absorbs ArF laser light is more easily decomposed.
- the binding energies in the S1 state of the N—C bond and the C—O bond part that are the starting points of the reaction were 366 kJ / mol and 269 kJ / mol, respectively. Since the polyimide resin has a sufficiently high binding energy in the S1 state, it is considered that gas generation is difficult to occur due to being hardly decomposed by ArF laser light.
- the energy of the S1 state of the O—C bond in O ⁇ C—O—C is a relatively small value of 63 kJ / mol, so that it can be said that the decomposition by ArF laser light was easily caused.
- the side chain O ⁇ CO is further cleaved with an activation energy of 74 kJ / mol to be eliminated as CO 2 . Since radicals are generated in the main chain portion, cleavage of the main chain tends to proceed. From these facts, it is considered that the acrylic resin easily generated gas by ArF laser light.
- the film containing the polyimide resin included in the pellicle frame of the present invention has excellent film strength and corrosion resistance while having good adhesion to metal. For this reason, generation
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Abstract
Description
[1]ペリクル膜の外周を支持するペリクルフレームであって、フレームと、前記フレームの表面に形成された、ポリイミド樹脂を含む膜と、を有するペリクルフレーム。
[3]前記ポリイミド樹脂を含む膜が、電着塗装膜である、[1]または[2]に記載のペリクルフレーム。
[4]前記電着塗装膜が、重縮合ポリイミド樹脂、熱架橋イミド樹脂、及びカチオン性ポリマーを含む組成物の硬化膜である、[3]に記載のペリクルフレーム。
[6]前記フレームが、黒色である、[1]~[5]のいずれかに記載のペリクルフレーム。
[7]ペリクル膜と、前記ペリクル膜の外周を支持する[1]~[6]のいずれか一項に記載のペリクルフレームと、を有する、ペリクル。
[8]ペリクル膜の外周を支持するペリクルフレームの製造方法であって、アルミニウム合金フレームを陽極酸化する工程と、前記アルミニウム合金フレ-ムの表面を黒色化処理する工程と、前記黒色化処理された前記アルミニウム合金フレームに、ポリイミド樹脂を含む塗料を塗装して、ポリイミド樹脂を含む膜を形成する工程と、を有する、ペリクルフレームの製造方法。
[9]ペリクル膜と、前記ペリクル膜の外周を支持するペリクルフレームと、を有するペリクルの製造方法であって、前記[8]に記載のペリクルフレームの製造方法で得られるペリクルフレームに、リソグラフィ用ペリクル膜を貼りつける工程を含む、ペリクルの製造方法。
本明細書において、「~」を用いて表される数値範囲は、「~」の前後に記載される数値を下限値及び上限値として含む範囲を意味する。
本発明のペリクルフレームは、フレームと、当該フレームの表面に形成された、ポリイミド樹脂を含む膜と、を有する。
以下、本発明のペリクルフレームのポリイミド樹脂を含む膜、及びフレームについて説明する。
本発明のペリクルフレームのフレームの形状は、ペリクルと貼り合わせるマスクの形状に合わせて適宜選択される。フレームの材質は、表面にポリイミド樹脂を含む膜を形成可能な金属であれば特に制限されず、その例には、アルミニウム、アルミニウム合金、マグネシウム合金、チタン、真鍮、鉄、ステンレス等が含まれる。中でもアルミニウム合金が、重量、加工性、耐久性等の観点から好ましい。また、アルミニウム合金からなるフレームは、電着塗装によりポリイミド樹脂を含む膜を容易に形成できるとの観点からも好ましい。
ポリイミド樹脂を含む膜は、フレ-ムの表面に形成された膜である。ポリイミド樹脂を含む膜の厚さは、好ましくは0.5μm以上30μm未満であり、より好ましくは5μm以上30μm未満であり、さらに好ましくは7μm以上25μm以下である。
スプレー塗装膜は、フレ-ムの表面にスプレー塗装法により形成した膜であって、ポリイミド樹脂を含む膜である。スプレー塗装法でポリイミド樹脂を含む膜を形成する場合、ポリイミドまたはその前駆体の濃度を希釈剤で調整後、スプレー塗装装置のスプレーノズルから、塗料を高圧空気とともに吹き付ける。そして、スプレーノズルから噴射された塗料の粒子を、上述のフレームに、均一に付着させ、必要に応じて加熱等を行って硬化させる。
電着塗装膜は、フレームの表面に電着塗装法により形成された膜であって、ポリイミド樹脂を含む膜である。電着塗装膜は、カチオン電着塗装法で形成された膜であってもよく、アニオン電着塗装法で形成された膜であってもよい。外観性が良好な膜、すなわち表面状態が平坦な塗装膜が得られるとの観点から、カチオン電着塗装法で形成された膜であることが好ましい。
カチオン電着塗装用組成物は、例えば、(A)ポリイミド樹脂と、(B)カチオン性ポリマーと、(C)中和剤と、(D)水性媒体とを含む組成物とすることができる。また、(A)ポリイミド樹脂及び(B)カチオン性ポリマーの代わりに、ポリイミド樹脂がカチオン変性された(A’)カチオン変性ポリイミド樹脂を含んでもよい。また、カチオン電着塗装用組成物は、必要に応じて(E)顔料や(F)その他の成分を含んでもよい。以下、これらの成分について説明する。
カチオン電着塗装用組成物が含むポリイミド樹脂は特に制限されない。(A)ポリイミド樹脂は、電着塗装膜の耐熱性や耐光性が高まるとの観点から、例えば下記一般式(1)で表される繰り返し単位を有する「重縮合ポリイミド樹脂」を含むことが好ましい。なお、本発明でいう「重縮合ポリイミド樹脂」とは、テトラカルボン酸二無水物とジアミンとを重縮合させて得られるポリイミド樹脂をいい、全芳香族ポリイミド類、全脂肪族ポリイミド類、半芳香族(半脂肪族)ポリイミド類のいずれかは問わない。ただし、重縮合ポリイミド樹脂に、後述の「熱架橋イミド樹脂」は含まないものとする。
(B)カチオン性ポリマーは、例えばアミノ基や、アミノ基の4級化塩等のカチオン性基を少なくとも1種含むポリマーであり得る。カチオン電着塗装用組成物が(B)カチオン性ポリマーを含む場合、前述の(A)ポリイミド樹脂に直接カチオン性基を導入しなくとも、(B)カチオン性ポリマーと(A)ポリイミド樹脂との相溶性等によって、(A)ポリイミド樹脂をフレーム表面に析出させることが可能となる。(B)カチオン性ポリマーは、例えばアクリル共重合体や、エポキシアミンアダクト樹脂等でありうる。
前述のように、カチオン電着塗装用組成物は、前述の(A)ポリイミド樹脂及び(B)カチオン性ポリマーの代わりに、(A’)カチオン変性ポリイミド樹脂を含んでもよい。カチオン電着塗装用組成物が、(A’)カチオン変性ポリイミド樹脂を含む場合、カチオン電着塗装用組成物に上述のアクリル樹脂やエポキシ樹脂等からなる(B)カチオン性ポリマーを別途含む必要がない。したがって、電着塗装膜の耐熱性がより高まりやすくなる。
カチオン電着塗装用組成物は、上述の(B)カチオン性ポリマーや、(A’)カチオン変性ポリイミド樹脂の水性媒体への分散性を向上させるための中和剤を含む。中和剤の例には、塩酸、硝酸、リン酸、ギ酸、酢酸、乳酸、コハク酸、酪酸のような無機酸または有機酸などが含まれる。中和剤は、カチオン電着塗装用組成物のpHが3~5の範囲となるように含まれることが好ましい。
カチオン電着塗装用組成物が含む水性媒体は、イオン交換水、純水などである。水性媒体は、必要に応じて、少量のアルコール類などを含んでもよい。カチオン塗装用組成物が含む(D)水性媒体の量は、カチオン塗装用組成物の粘度等に応じて適宜選択される。
カチオン電着塗装用組成物は、カーボンブラック等の顔料を含んでもよい。ペリクルフレームが、カチオン電着塗装膜により黒色化されると、前述のようにペリクルフレーム表面に付着した塵埃を確認しやすくなる。
カチオン電着塗装用組成物は、必要に応じて、他の成分を含んでもよい。他の成分の例には、水混和性有機溶剤、界面活性剤、酸化防止剤、紫外線吸収剤などが含まれる。
電着塗装膜は、1)フレーム表面に、前述のカチオン性電着塗装用組成物の膜を形成する工程と、2)得られた膜を加熱硬化および乾燥させて硬化電着塗装膜とする工程と、により形成される。
前述のように、本発明のペリクルフレームは、フレームを作製し、当該フレーム上に、ポリイミド樹脂を含む膜を形成することで製造することができる。ペリクルフレームの製造方法は、フレームの種類や、ポリイミド樹脂を有する膜の形成方法等に応じて適宜選択することができる。
本発明のペリクルは、ペリクル膜と、前記ペリクル膜の外周を支持する前述のペリクルフレームと、前記ペリクルフレームと前記ペリクル膜とを接着させる膜接着剤と、前記ペリクルフレームと前記マスクとを接着するためのマスク接着剤とを有する。図1には、本発明のペリクルの一例が示される。ペリクル10は、ペリクル膜12と、ペリクル膜12の外周を支持するペリクルフレーム14とを有する。ペリクル膜12は、ペリクルフレーム14の一方の端面にある膜接着剤層13を介して張設されている。一方、ペリクルフレーム14をマスク(不図示)に接着させるために、ペリクルフレーム14のもう一方の端面には、マスク接着剤層15が設けられている。
JIS A7075-T6製のアルミニウムフレーム(寸法:149mm×122mm×高さ5.8mm、支持枠厚さ2mm)を用意した。当該フレームを大気中、温度250℃で20分間焼鈍した。その後、平均直径約100μmのステンレスにて、フレーム表面をショットブラスト処理した。
次いで、15質量%の硫酸の電解浴を用い、電解電圧20V、電気量10C/cm2にて当該フレームを陽極酸化した。その後、硫酸ニッケル六水和物160g/L、ホウ酸40g/L、酒石酸3g/L、及び酸化マグネシウム1g/Lが溶解した電解析出浴を用い、30℃、交流電圧15Vの定電圧電解にて、電解析出処理を6分間行った。これにより、着色したフレームが得られた。
そして、フレームを純水にて洗浄し、カチオン系ポリイミド電着塗料((株)シミズ製 エレコートPI)の入った浴槽に入れ、25℃、電圧100Vで1分間電着塗装した。電着塗装後のフレームを水洗し、100℃で15分乾燥後、180℃、30分間焼付を実施して、フレーム上に厚さ10μmの電着塗装膜(ポリイミド樹脂を含む膜)が形成されたペリクルフレーム1を得た。
陽極酸化処理及び電着塗装を以下の条件で行った以外は、実施例1と同様にペリクルフレーム2を作製した。
酒石酸ナトリウム二水和物53g/L、及び水酸化ナトリウム4g/Lが溶解したアルカリ性水溶液を電解液とし、5℃、電解電圧30V、電気量10C/cm2の条件で陽極酸化を行った。
電解析出処理後のフレームを純水で洗浄し、カチオン系ポリイミド電着塗料((株)シミズ製 エレコートPI)の入った浴槽に入れた。そして、陽極にカーボン板、陰極にフレームを使用し、25℃、電圧100Vで1分電着塗装した。その後、実施例1と同様に水洗、乾燥、及び焼き付けを実施し、厚さ9μmの電着塗装膜(ポリイミド樹脂を含む膜)を得た。
枠型形状をなす外形寸法148.95mm×114.95mm×厚さ2.50mmのアルミ合金7075製フレーム材に、以下の条件で陽極酸化処理を行った。その後、実施例2と同様の電着塗装を行い、厚さ5~20μmの電着塗装膜(ポリイミド樹脂を含む膜)が形成されたペリクルフレーム3を作製した。
無機酸水和物を溶解したアルカリ性水溶液を電解液とし、pH12~14の溶液を用い、浴温度を0~20℃にて、電圧を0.5V以上20V未満、処理時間を2~120分の条件で陽極酸化を行った。
枠型形状をなす外形寸法148.95mm×114.95mm×厚さ2.50mmのアルミ合金7075製フレーム材に、実施例3と同様に陽極酸化処理を施した。その後、(株)ピーアイ技術研究所製のアニオン系ポリイミド電着塗料を電着塗装し、厚さ5~20μmの電着塗装膜(ポリイミド樹脂を含む膜)が形成されたペリクルフレーム4を作製した。
ペリクルフレーム4の外観を目視で確認したところ、ペリクルフレーム4の電着塗装膜(ポリイミド樹脂を含む膜)は、ペリクルフレーム3の電着塗装膜(ポリイミド樹脂を含む膜)よりも塗膜の表面状態が粗かった。
実施例3と同様に、フレーム材に陽極酸化処理を同様に施した。その後、(株)IST製のポリイミド塗料を、希釈溶剤で希釈した。そして、当該塗料をスプレー塗装し、厚さ0.5~20μmのスプレー塗装膜(ポリイミド樹脂を含む膜)が形成されたペリクルフレーム5を作製した。
電着塗装の代わりに、以下の条件で封孔処理した以外は、実施例1と同様にペリクルフレーム6を作製した。
電解析出処理後のフレームを、蒸気封孔装置にいれ、相対湿度100%、2.0kg/cm2G、130℃の水蒸気を発生させながら30分間封孔処理を行った。
電着塗装の代わりに、以下の条件で封孔処理した以外は、実施例2と同様にペリクルフレーム7を作製した。
(封孔処理)
電解析出処理後のフレームを、蒸気封孔装置にいれ、相対湿度100%、2.0kg/cm2G、130℃の水蒸気を発生させながら30分間封孔処理を行った。
電着塗装時に、カチオン系ポリイミド電着塗料((株)シミズ製 エレコートPI)の代わりに、アクリル系樹脂電着塗料((株)シミズ製 エレコート ナイスロン)を使用し、陰極にカーボン板、陽極にフレームを使用した以外は、実施例1と同様に、ペリクルフレーム8を作製した。このとき、電着塗装膜(アクリル系樹脂を含む膜)の厚さは10μmであった。
1)発生ガス量の評価
実施例1、5、及び比較例3で作成したペリクルフレームを各々4cm程度に切断し、測定用サンプルを作製した。各測定用サンプルをそれぞれ2口のスクリューキャップが付いた太鼓型石英セルに入れ、1つのスクリューキャップに窒素を流すラインを取り付け、窒素を100mL/minで流した。さらにもう1つのスクリューキャップに捕集管(ジーエルサイエンス製TRAP TUBE、TENAX GL)を取り付けた。窒素を使用するのは、酸素があるとArFレーザにより酸素がオゾンに変化し、オゾンによって補修管中の捕集材が劣化するため、サンプルから発生するガスが捕集できなくなることを防ぐためである。
スクリューキャップ内を完全に窒素置換後、太鼓型石英セル内の測定用サンプルにArFレーザを1000Hz、0.4mJ/cm2の条件で5分間照射した。
ArFレーザ照射により、測定用サンプル表面からガスとなって脱離した物質を捕集管に採取し、発生ガスサンプルを得た。
次いで、加熱脱着ガスクロマトグラフ質量分析計(GC-MS)を用いて捕集管で採取した物質量を発生ガス量(ウンデカン換算)として測定した。測定には株式会社島津製作所製の加熱脱着GC-MS(TDTS-2010)、ガスクロマトグラフ(GC-2010)、質量分析計(GCMS-QP2010)を使用した。結果を表1に示す。
旭化成株式会社製のジッパー付き耐熱袋(ジップロック(登録商標))に、100mlの超純水を入れた。これに、実施例1~5、および比較例1、2で作製したペリクルフレーム毎に、ペリクルフレームを3枚ずつ入れて空気を抜き、ジッパーで密閉した。この耐熱袋を、90℃の高温水槽に3時間浸漬して、ペリクルフレームに含まれる各種イオンを抽出した。抽出液に含まれる各種イオン量を、イオンクロマトグラフ分析装置(DIONEX Corporation製ICS-1000(カラム:AS9-HC))により測定した。このとき、溶離液は1mmol/LのK2CO3溶液とした。各ペリクルフレームから溶出されたイオンの種類及びその量を表2に示す。
12 ペリクル膜
13 膜接着剤層
14 ペリクルフレーム
15 マスク接着剤層
Claims (9)
- ペリクル膜の外周を支持するペリクルフレームであって、
フレームと、前記フレームの表面に形成された、ポリイミド樹脂を含む膜と、を有するペリクルフレーム。 - 前記フレームは、陽極酸化処理されたアルミニウム合金フレームである、請求項1に記載のペリクルフレーム。
- 前記ポリイミド樹脂を含む膜が、電着塗装膜である、請求項1または2に記載のペリクルフレーム。
- 前記電着塗装膜が、重縮合ポリイミド樹脂、熱架橋イミド樹脂、及びカチオン性ポリマーを含む組成物の硬化膜である、請求項3に記載のペリクルフレーム。
- 前記ポリイミド樹脂を含む膜の厚さが、25μm以下である、請求項1~4のいずれか一項に記載のペリクルフレーム。
- 前記フレームが、黒色である、請求項1~5のいずれか一項に記載のペリクルフレーム。
- ペリクル膜と、
前記ペリクル膜の外周を支持する請求項1~6のいずれか一項に記載のペリクルフレームと、
を有する、ペリクル。 - ペリクル膜の外周を支持するペリクルフレームの製造方法であって、
アルミニウム合金フレームを陽極酸化する工程と、
前記アルミニウム合金フレ-ムの表面を黒色化処理する工程と、
前記黒色化処理された前記アルミニウム合金フレームに、ポリイミド樹脂を含む塗料を塗装して、ポリイミド樹脂を含む膜を形成する工程と、
を有する、ペリクルフレームの製造方法。 - ペリクル膜と、前記ペリクル膜の外周を支持するペリクルフレームと、を有するペリクルの製造方法であって、
請求項8に記載のペリクルフレームの製造方法で得られるペリクルフレームに、ペリクル膜を貼りつける工程を含む、
ペリクルの製造方法。
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JP2021144249A (ja) * | 2017-10-10 | 2021-09-24 | 信越化学工業株式会社 | 半導体デバイスまたは液晶ディスプレイの製造方法 |
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CN110347013A (zh) * | 2018-04-03 | 2019-10-18 | 信越化学工业株式会社 | 蒙版框架、蒙版和蒙版框架的制备方法 |
US11003070B2 (en) | 2018-04-03 | 2021-05-11 | Shin-Etsu Chemical Co., Ltd. | Pellicle frame, pellicle, and method of producing pellicle frame |
JP7139133B2 (ja) | 2018-04-03 | 2022-09-20 | 信越化学工業株式会社 | ペリクルフレーム、ペリクル、及びペリクルフレームの製造方法 |
US11474427B2 (en) | 2018-04-03 | 2022-10-18 | Shin-Etsu Chemical Co., Ltd. | Pellicle frame, pellicle, and method of producing pellicle frame |
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Publication number | Publication date |
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EP3339955A1 (en) | 2018-06-27 |
EP3339955B1 (en) | 2020-05-20 |
EP3339955A4 (en) | 2019-03-06 |
US10606169B2 (en) | 2020-03-31 |
TW201712428A (zh) | 2017-04-01 |
JP6548339B2 (ja) | 2019-07-24 |
TWI726901B (zh) | 2021-05-11 |
JP6551837B2 (ja) | 2019-07-31 |
JP2018028659A (ja) | 2018-02-22 |
JP2017040688A (ja) | 2017-02-23 |
KR20180030133A (ko) | 2018-03-21 |
US20180239242A1 (en) | 2018-08-23 |
KR102079989B1 (ko) | 2020-02-24 |
CN107924117A (zh) | 2018-04-17 |
CN107924117B (zh) | 2021-05-18 |
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