CN1934496B - Photosensitive insulative paste composition and photosensitive film using the same - Google Patents
Photosensitive insulative paste composition and photosensitive film using the same Download PDFInfo
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- CN1934496B CN1934496B CN200580009109.0A CN200580009109A CN1934496B CN 1934496 B CN1934496 B CN 1934496B CN 200580009109 A CN200580009109 A CN 200580009109A CN 1934496 B CN1934496 B CN 1934496B
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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
- G03F7/00—Photomechanical, e.g. photolithographic, production of textured or patterned surfaces, e.g. printing surfaces; Materials therefor, e.g. comprising photoresists; Apparatus specially adapted therefor
- G03F7/004—Photosensitive materials
- G03F7/0047—Photosensitive materials characterised by additives for obtaining a metallic or ceramic pattern, e.g. by firing
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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
- G03F7/00—Photomechanical, e.g. photolithographic, production of textured or patterned surfaces, e.g. printing surfaces; Materials therefor, e.g. comprising photoresists; Apparatus specially adapted therefor
- G03F7/004—Photosensitive materials
- G03F7/0046—Photosensitive materials with perfluoro compounds, e.g. for dry lithography
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
- H01J11/00—Gas-filled discharge tubes with alternating current induction of the discharge, e.g. alternating current plasma display panels [AC-PDP]; Gas-filled discharge tubes without any main electrode inside the vessel; Gas-filled discharge tubes with at least one main electrode outside the vessel
- H01J11/20—Constructional details
- H01J11/22—Electrodes, e.g. special shape, material or configuration
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
- H01J11/00—Gas-filled discharge tubes with alternating current induction of the discharge, e.g. alternating current plasma display panels [AC-PDP]; Gas-filled discharge tubes without any main electrode inside the vessel; Gas-filled discharge tubes with at least one main electrode outside the vessel
- H01J11/20—Constructional details
- H01J11/34—Vessels, containers or parts thereof, e.g. substrates
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
- H01J11/00—Gas-filled discharge tubes with alternating current induction of the discharge, e.g. alternating current plasma display panels [AC-PDP]; Gas-filled discharge tubes without any main electrode inside the vessel; Gas-filled discharge tubes with at least one main electrode outside the vessel
- H01J11/20—Constructional details
- H01J11/34—Vessels, containers or parts thereof, e.g. substrates
- H01J11/36—Spacers, barriers, ribs, partitions or the like
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
- H01J9/00—Apparatus or processes specially adapted for the manufacture, installation, removal, maintenance of electric discharge tubes, discharge lamps, or parts thereof; Recovery of material from discharge tubes or lamps
- H01J9/02—Manufacture of electrodes or electrode systems
Abstract
A photosensitive insulative paste composition that can be developed in an alkaline developer or water and can be used to form a thick but still highly sensitive layer and, thus, high-precision patterns. The photosensitive insulative paste composition contains an organic component and an inorganic powder and the organic component comprises (A) a water-soluble cellulose derivative, (B) a hydroxyl-containing acrylic resin having a molecular weight of 20000 or less, (C) a photopolymerizable monomer, and (D) a photopolymerization initiator.
Description
Technical field
The present invention relates to photosensitive insulative paste composition and corresponding photosensitive film.Particularly, the present invention relates to a kind of photosensitive insulative paste composition,, and contain inorganic powder and, still can guarantee to form high-precision patterns the organic component of development high-resistance even in thick rete with enough high photosensitivities.The present invention also relates to use the photosensitive film of this photosensitive insulative paste composition.
Background technology
When producing the construction package of thick multilayer circuit and various display pannels, use for example screen printing technique and photoetching process usually.In serigraphy, required pattern be to use the photohardenable insulative paste that contains inorganic particles and wire mark on base material.In photoetching process, see through photomask with the activation ray and shine the photohardenable insulative paste composition that is coated on the base material, for example ultraviolet ray makes required pattern development on base material.
In dissimilar display pannels, plasm display panel (after this Plasma DisplayPanels abbreviates " PDPs " as) has simple relatively structure, therefore is suitable for roomy display.PDPs is (light) emissivity device, and what can show is not high quality graphic, but the suitable high quality graphic of color.Because these are favourable, PDPs obviously receives publicity, and people make various schemes, makes great efforts the bigger plasma scope that can show precise image of research and development.
A PDP contains two groups of relative base materials, and the barrier (barrier ribs) with insulation has surrounded a large amount of display units therebetween.Work as a pixel in each unit, it contains fluorescent material, shines following time by the ultraviolet ray of plasma exciatiaon and can launch light being exposed to.The assembly that electrode, resistance, dielectric and other produce plasma is arranged on the base material or in the unit.In order to construct the PDP of high precision, the barrier that its assembly comprises, electrode, resistance, dielectric, fluorescent material, color filter, and black matrix" (Black Matrices) needs accurately to make up (after this assembly all is referred to as " barrier or analog "), and therefore, the pattern that is used to form barrier or analog also needs accurately to make up.
In traditional screen printing technique, predetermined paste composition pattern is connect one deck by one deck and is printed on another layer, forms multilayer pattern.Will aim at these patterns exactly, it is difficult forming high-precision barrier.Photoetching technique has its shortcoming equally: the photonasty that is used to form the thick film layers of barrier or analog can tend to weaken with the degree of depth.This also makes the formation high-precision patterns become difficult.In addition, photoetching process needs expensive organic solvents, and for example trichloroethanes is as developer.This has increased production cost.These solvents also cause environmental pollution, and are harmful to health.
In order to solve these problems relevant, a kind of photohardenable insulative paste composition that can develop has been proposed in aqueous solution with development step with an organic solvent.This composition contains for example water-soluble cellulose of methylcellulose, photopolymerizable monomer, Photoepolymerizationinitiater initiater, and inorganic powder (example is seen patent documentation 1 (Japanese patent application publication No. No.Sho63-265238)).Yet this composition has repellence to development by halves.Therefore proposed a kind of photosensitive insulative paste composition that can head it off, this composition has also solved in the serigraphy, forms inaccurate problem owing to decompose the barrier that image-region and formation of barrier ribs cause.This composition contains water-soluble cellulose derivative, photopolymerizable monomer, the acryl resin of hydroxyl, Photoepolymerizationinitiater initiater, and inorganic powder (example is seen patent documentation 2 (Japanese patent application publication No. No.200263-328470)).
Summary of the invention
Yet, the photosensitive insulative paste composition of describing in the patent documentation 2, if for the total amount (=100 weight portion) after hydrophobic acrylic acid's resin merging of water-soluble cellulose derivative and hydroxyl, wherein hydrophobic acrylic acid's resin of hydroxyl is 50 weight portions or more, can form residue in development step.The adding of this acryl resin makes composition to development more repellence be arranged, and this kind residue will influence developing manufacture process.
Standing state for technology, the present inventor is devoted to find out solution to the problems described above in a large number, find at last, as long as the molecular weight of the acryl resin of hydroxyl does not exceed 20000, just can not hinder developing manufacture process, even it contains the acryl resin (merge for water-soluble cellulose derivative and hydroxy acryl acid resin after total amount (=100 weight portion)) of 90 to 50 weight portion hydroxyls, and the developer resistance in the composition can be improved by acryl resin content to 50 weight portion or higher (merge for water-soluble cellulose derivative and the hydroxy acryl acid resin after total amount (=100 weight portion)) that adjustment has a hydroxyl.The present invention promptly is based on this discovery.
One object of the present invention is to provide a kind of insulative paste composition of photosensitivity, even contain a large amount of hydrophobic resin components, also can in alkaline developer or water, develop, can form thick but the rete raw material of hypersensitivity, therefore be suitable for high-precision patterns.Another object of the present invention is to provide a kind of photosensitive film that uses this kind photosensitive insulative paste composition.
Photosensitive insulative paste composition of the present invention comprises a kind of organic component and a kind of inorganic powder.Described organic component comprises (A) water-soluble cellulose derivative, and (B) molecular weight of hydroxyl is 20000 or lower acryl resin, (C) photo polymerization monomer and (D) Photoepolymerizationinitiater initiater.Preferably, for the total amount (=100 weight portion) after component in the organic component (A) and component (B) merging, the amount that described photosensitive insulative paste composition comprises component (A) and component (B) is respectively 10 to 50 weight portions and 90 to 50 weight portions.
Preferably, the inorganic powder that is used for photosensitive insulative paste composition of the present invention is a kind of glass powder, for the total amount (=100 weight portion) after component in the organic component (A) and component (C) merging, the amount that described photosensitive insulative paste composition comprises component (A) and component (C) is respectively 10 to 50 weight portions and 90 to 50 weight portions.
Preferably, the total amount (=100 weight portion) after merging for organic component that photosensitive insulative paste composition of the present invention comprised and inorganic powder, their content is respectively 5 to 35 weight portions and 95 to 65 weight portions.
Photosensitive film of the present invention is characterised in that above-mentioned photosensitive insulative paste composition rete is formed on the supporting film.
Photosensitive insulative paste composition of the present invention is used in the water or carries out high-precision patterns in the alkaline developer when developing, and shows good performance: this kind composition can be used for forming thick and still has the high precision insulating layer pattern of high photosensitivity.Therefore, photosensitive insulative paste composition of the present invention can have essential industry and be worth high precision PDPs with low-cost production.
Preferred forms of the present invention
Below will introduce one exemplary embodiment of the present invention.
Photosensitive insulative paste composition of the present invention comprises a kind of organic component and a kind of inorganic powder.Described organic component comprises (A) water-soluble cellulose derivative, and (B) molecular weight of hydroxyl is 20000 or lower acryl resin, (C) photo polymerization monomer and (D) Photoepolymerizationinitiater initiater.
Photosensitive insulative paste composition of the present invention contains the water soluble dyes derivant as bonding resin, compare with traditional photosensitive insulative paste composition based on acryl resin, it is for ultraviolet ray, laser, the X-ray, electron beam and other activation ray have all shown high transmittance and development have been had higher repellence.So composition of the present invention can form the pattern of pin-point accuracy.
Photosensitive insulative paste composition of the present invention use the molecular weight with hydroxyl be 20000 or lower acryl resin as component (B), make it be unlikely to disturb development step, even for water-soluble cellulose derivative and acryl resin merging amount (=100 weight portions with hydroxyl, after this be referred to as " resin Composition total amount "), wherein the content of component (B) is 50 weight portions or more.Equally, for resin Composition total amount (=100 weight portion), by regulating component (B), the content of hydrophobic resin is 50 weight portions or more, and described paste composition can show the development property of improvement.
Water-soluble cellulose derivative as component (A) can be any known water-soluble cellulose derivative, comprises carboxymethyl cellulose, hydroxyethyl cellulose, HEMC, hydroxypropyl cellulose, ethylhydroxyethylcellulose, carboxymethylethylcellulose and hydroxypropyl methylcellulose.These cellulose derivatives both can separately be used, and also can be used as the potpourri of two or more derivants and used.
Usually have 20000 or lower molecular weight as the acryl resin with hydroxyl of component (B), be preferably 5000 to 15000, more preferably 8000 to 12000.Molecular weight as fruit component (B) exceeds 20000, and for water-soluble cellulose derivative with have an acryl resin merging amount (=100 weight portion) of hydroxyl, acryl resin content with hydroxyl is 50 weight portions or more, the development property of composition may reduce, and may form unnecessary residue.
Acryl resin with hydroxyl can be a kind of multipolymer, and the monomer by having hydroxyl gets through polyreaction as main copolymerizable monomer.If necessary, can use other can with the monomer of monomer copolymerization with hydroxyl.
Preferred embodiment with carboxylic monomer is that acrylic acid or methacrylic acid and the single alcohol that contains 1 to 20 carbon atom react formed monoesters, comprises acrylic acid hydroxyl methyl esters, hydroxy methyl methacrylate, acrylic acid 2-hydroxyl ethyl ester, methacrylic acid 2-hydroxyethyl ester, acrylic acid 2-hydroxypropyl ester, methacrylic acid 2-hydroxypropyl ester, acrylic acid 3-hydroxypropyl acrylate, methacrylic acid 3-hydroxypropyl ester, acrylic acid 2-hydroxy butyl ester, methacrylic acid 2-hydroxyl butyl ester, acrylic acid 3-hydroxy butyl ester, methacrylic acid 3-hydroxyl butyl ester, acrylic acid 4-hydroxy butyl ester, methacrylic acid 4-hydroxyl butyl ester.
Other preferred embodiment with monomer of hydroxyl comprises the monoesters of acrylic acid or methacrylic acid and the diol reaction formation that contains 1 to 10 carbon atom, and epoxy ester compounds, comprise the hydroxy-ethyl acrylate of acrylic acid glyceride, glyceral methacrylate, single acrylic acid dipentaerythritol ester, monomethyl acrylic acid dipentaerythritol ester, 6-caprolactone modification, hydroxyethyl methylacrylate and the 2-hydroxyl-3-phenoxy propyl acrylate that 6-caprolactone is modified.
The preferred embodiment of other monomer can with the monomer copolymerization with hydroxyl, comprise α, beta-unsaturated carboxylic acid, for example acrylic acid, methacrylic acid, itaconic acid, citraconic acid, maleic acid and fumaric acid, and acid anhydrides and half ester product thereof; α, the formed ester of beta-unsaturated carboxylic acid, methyl acrylate for example, ethyl acrylate, the acrylic acid n-propyl, isopropyl acrylate, n-butyl acrylate, isobutyl acrylate, sec-butyl acrylate, cyclohexyl acrylate, acrylic acid-2-b hexyl, acrylic acid octadecane ester, methyl methacrylate, Jia Jibingxisuanyizhi, n propyl methacrylate, isopropyl methacrylate, the secondary propyl ester of methacrylic acid, n-BMA, isobutyl methacrylate, the secondary butyl ester of methacrylic acid, cyclohexyl methacrylate, methacrylic acid-2-b hexyl, methacrylic acid octadecane ester, acrylic acid 2,2,2-trifluoro methyl esters, with methacrylic acid 2,2,2-trifluoro methyl esters; And styrene compound, for example styrene, α-Jia Jibenyixi, p-methylstyrene.Other example comprises vinyl cyanide, methacrylonitrile, acrylamide, Methacrylamide, vinyl acetate, glycidyl acrylate and glycidyl methacrylate.These compounds both can separately use, and also can be used as the potpourri of two or more compounds and used.
For the total amount (=100 weight portion) of resin Composition, the acryl resin with hydroxyl that photosensitive insulative paste composition of the present invention is contained is advisable with 50 to 90 weight portions, 60 to 80 weight portions more preferably, 65 to 75 weight portions more preferably again.
If the acrylic resin component content with hydroxyl is not in the scope of defined, the pattern that obtains at last might not reach the degree of accuracy that needs: the acryl resin with hydroxyl that is lower than 50 weight portions may cause the developer barrier properties to reduce, yet the described resin that is higher than 90 weight portions has and causes development property downward trend, and can form unnecessary residue at developing process.For example, the amount of photopolymerizable monomer is lower than 50 weight portions can cause the photopolymerization reaction deficiency, thereby causes image-region decomposition in the development step, promptly can not form image.In contrast, the amount of photopolymerizable monomer is higher than the resolution decline that 90 weight portions can cause precise image.
Photopolymerizable monomer as component (C) can be any known photopolymerizable monomer, include, but are not limited to, ethylene glycol diacrylate, Ethylene glycol dimethacrylate, the diacrylate triethyleneglycol ester, the dimethacrylate triethyleneglycol ester, trimethylolpropane triacrylate, trimethylol-propane trimethacrylate, the trimethylolethane trimethacrylate acrylate, the trimethylolethane trimethacrylate methacrylate, the diacrylate pentaerythritol ester, the dimethacrylate pentaerythritol ester, pentaerythritol triacrylate, trimethyl acrylic acid pentaerythritol ester, pentaerythritol tetracrylate, pentaerythritol tetramethacrylate, dipentaerythritoltetraacrylate, tetramethyl acrylic acid dipentaerythritol ester, five acrylic acid dipentaerythritol ester, pentamethyl acrylic acid dipentaerythritol ester, six acrylic acid dipentaerythritol ester, hexamethyl acrylic acid dipentaerythritol ester, the acrylic acid glycerine ester, the methacrylic acid glycerine ester, with Cardo type epoxy diacrylate, and fumarate, itaconate and maleate, they are respectively to use fumaric acid, itaconic acid and maleic acid are replaced (methyl) acrylic acid of above-claimed cpd and are got.
Photoepolymerizationinitiater initiater as component (D) can be any common Photoepolymerizationinitiater initiater, comprises Benzophenones, diphenylhydroxyethanone class, diphenylhydroxyethanone alkyl ether, acetophenone class, aminoacenaphthene class, benzyl class, benzyl alkyl ketal class, anthraquinone class, ketal class and thioxanthene ketone.Clear and definite example can comprise 2; triazine between two trichloromethyl-6-(the 3-bromo-4-methoxyl) phenyl of 4-; 2; triazine between two trichloromethyl-6-(the 2-bromo-4-methoxyl) phenyl of 4-; 2; triazine between two trichloromethyl-6-(3-bromo-4-methoxyl) the styryl phenyl of 4-; 2; triazine between two trichloromethyl-6-(2-bromo-4-methoxyl) the styryl phenyl of 4-; 2; 4; 6-trimethylbenzene formyl diphenyl phosphine oxide; 1-[4-(2-hydroxy ethoxy) phenyl]-2-hydroxy-2-methyl-1-propane-1-ketone; 2; the 4-diethyl thioxanthone; 2; 4-dimethyl thioxanthones; the 2-clopenthixal ketone; 1-chloro-4-propoxyl group thioxanthones; 3; 3-dimethyl-4-methoxyl benzophenone; benzophenone; 1-(4-isopropyl phenyl)-2-hydroxy-2-methyl propane-1-ketone; 1-(4-dodecylphenyl)-2-hydroxy-2-methyl propane-1-ketone; 4-benzoyl-4 '-methyl dimethoxy base sulphur; 4-dimethylaminobenzoic acid ester; 4-dimethylaminobenzoic acid methyl esters; 4-dimethylaminobenzoic acid ethyl ester; 4-dimethylaminobenzoic acid butyl ester; 4-dimethylaminobenzoic acid 2-b hexyl; 4-dimethylaminobenzoic acid 2-isopentyl ester; 2; the 2-diethoxy acetophenone; the benzyl dimethyl ketal; benzyl-beta-methoxy-ethyl acetal; 1-phenyl-1; 2-propanedione-2-(adjacent ethoxy carbonyl) oxime; o-benzoyl yl benzoic acid methyl esters; two (4-dimethylamino phenyl) ketone; 4; 4 '-two lignocaine benzophenone; benzyl; diphenylhydroxyethanone; the diphenylhydroxyethanone methyl ether; the diphenylhydroxyethanone ethylether; the diphenylhydroxyethanone isopropyl ether; the diphenylhydroxyethanone n-butyl ether; the diphenylhydroxyethanone isobutyl ether; right-the dimethylamino acetophenone; right-tert-butyl group trichloroacetophenone; right-tert-butyl group dichloroacetophenone; thioxanthones; 2-methyl thioxanthones; the 2-isopropyl thioxanthone; Dibenzosuberone; α; α-Er Lv-4-Ben Yangjibenyitong; 4-dimethylaminobenzoic acid pentyl ester; and 2-(Chloro-O-Phenyl)-4,5-diphenyl-imidazole base dipolymer.These compounds both can separately use, and also can be used as the potpourri of two or more compounds and used.
For the merging amount (=100 weight portion) of water-soluble cellulose derivative and photopolymerizable monomer, the Photoepolymerizationinitiater initiater preferable amount is 0.1 to 10 weight portion, more preferably 0.2 to 5 weight portion.The amount of Photoepolymerizationinitiater initiater is less than 0.1 weight portion may cause that curing performance descends, otherwise if Photoepolymerizationinitiater initiater content more than 10 weight portions, just may absorb light before light arrives the bottom, it is not enough to cause its place to be solidified.
In component (A) to component (D), photosensitive insulative paste composition of the present invention can comprise optional adjuvant, for example ultraviolet light absorber, sensitizer, auxiliary sensitizer, polymerization inhibitor, plastifier, viscosifying agent, organic solvent, spreading agent, foam reducing composition, inorganic or organic supensoid agent.
The purpose of adding sensitizer is to increase photosensitivity.The instantiation of sensitizer comprises 2, the 4-diethyl thioxanthone, isopropyl thioxanthone, 2, two (the 4-lignocaine benzylidene) cyclopentanone of 3-, 2, two (the 4-dimethylamino benzylidene) cyclohexanone of 6-, 2, two (4-dimethylamino the benzylidene)-4-methyl cyclohexanones of 6-, Michaelis (Michler) ketone, 4, two (the lignocaine)-benzophenone of 4-, 4, two (dimethylamino) chalcone of 4-, 4, two (lignocaine) chalcone of 4-, to dimethylamino cinnamylidene indone, to Dimethylaminobenzene methylene indone, 2-(to the Dimethylaminobenzene ethenylidene)-different naphthothiazoles, 1, two (the 4-dimethylamino benzylidene) acetone of 3-, 1,3-carbonyl-two (4-lignocaine benzylidene) acetone, 3,3-carbonyl-two (7-lignocaine cumarin), N-phenyl-N-ehtylethanolamine, the N-phenylethanol amine, N-tolyl diethanolamine, the N-phenylethanol amine, the dimethylaminobenzoic acid isopentyl ester, the lignocaine isoamyl benzoate, 3-phenyl-5-benzoyl s-based tetrazolium, with 1-phenyl-5-ethoxy carbonyl s-based tetrazolium.These sensitizers both can use individually, also can two or more mix use.
In order to increase the thermal stability in the storage process, can add polymerization inhibitor, its particular instance can comprise monoesters, N nitrosodiphenyl amine, phenothiazine, p-tert-butyl catechol, the N-nonox, 2 of p-dihydroxy-benzene, p-dihydroxy-benzene, 6-di-tert-butyl methyl phenol, tetrachloroquinone and 1,2,3,-thrihydroxy-benzene.
In order to increase the compliance with base material, can add plastifier, its particular instance can comprise phthalate, for example dibutyl phthalate (DBP), dioctyl phthalate (DOP) and dicyclohexyl phthalate, also can be polyglycol, glycerine and dibutyl tartrate.
Foam reducing composition is used for preventing that lotion or film from forming foam, and described foam causes aperture to form after oven dry.The particular instance of foam reducing composition can comprise the material based on alkylene glycol, polyglycol (molecular weight=400 are to 800) for example, type siloxane, or more senior alcohols.
In the photosensitive insulative paste composition of the present invention, inorganic powder can be to the enough transparent any inorganic powder of light source.The example can comprise glass, pottery (for example, trichroite) and metal powder.Example can be the powder of borosilicate lead glass, borosilicate zinc glass and borosilicate bismuth glass, for example PbO-SiO more specifically
2Glass, PbO-B
2O
3-SiO
2Glass, ZnO-SiO
2Glass, ZnO-B
2O
3-SiO
2Glass, BiO-SiO
2Glass and BiO-B
2O
3-SiO
2Glass; The oxide powder of Na, K, Mg, Ca, Ba, Ti, Zr and Al, for example cobalt oxide, iron oxide, chromium oxide, nickel oxide, cupric oxide, manganese oxide, neodymia, vanadium oxide, cerium oxide, titan yellow, cadmium oxide, ruthenium-oxide, silicon dioxide, magnesium oxide and spinel; Fluorescent material powder, for example ZnO:Zn, Zn
3(PO
4)
2: Mn, Y
2SiO
5: Ce, CaWO
4: Pb, BaMgAl
14O
23: Eu, ZnS:(Ag, Cd), Y
2O
3: Eu, Y
2SiO
5: Eu, Y
3Al
5O
12: Eu, YBO
3: Eu, (Y, Gd) BO
3: Eu, GdBO
3: Eu, ScBO
3: Eu, LuBo
3: Eu, Zn
2SiO
4: Mn, BaAl
12O
19: Mn, SrAl
13O
19: Mn, CaAl
12O
19: Mn, YBO
3: Tb, BaMgAl
14O
23: Mn, LuBO
3: Tb, GdBO:Tb, ScBO
3: Tb, Sr
6Si
3O
3Cl
4: Eu, ZnS:(Cu, Al), ZnS:Ag, Y
2O
2S:Eu, ZnS:Zn, (Y, Cd) BO
3: Eu and BaMgAl
12O
23: Eu; And metal powder, for example iron, nickel, palladium, tungsten, copper, aluminium, silver, gold and platinum.In these materials, glass powder and ceramic powders are particularly preferred, because they have the high grade of transparency.Glass powder (glass dust) has the most significant effect.Preferably, inorganic powder oxygen-free silicon, aluminium oxide, or titanium dioxide, because these compounds make inorganic powder opaque, and the transmittance of reduction inorganic powder.
Inorganic powder preferably has the average particle size particle size of 0.5 to 10 μ m, and although 1 to 8 μ m more preferably is the pattern contour that described size can form as required and changing.Average particle size particle size can cause forming rough surface greater than the inorganic powder of 10 μ m when forming high-precision patterns, otherwise average particle size particle size stops light to be penetrated into the bottom downwards less than the inorganic powder meeting scattered beam of 0.5 μ m.Inorganic powder can have various profiles, and is for example spherical, piece shape, and thin slice shape or branch shape, and can present in these profiles one or more.
Inorganic powder not only comprises black powder, also comprises the inorganic pigment of different colours, and is for example red, blueness, and green pigment.The photosensitive insulative paste composition that comprises this pigment can be used for forming the pattern of different colours, therefore is suitable for producing the assembly of color filter or other plasma display panel.Described inorganic powder can be the potpourri of multiple subparticle, and each particle all has different physical attributes.Have the glass powder or the ceramic powders of different thermal softening points by use, the contraction that produces during oven dry can minimize.These inorganic powders can a kind of suitable shape and the physical attribute array mode mix, its physical attribute and required barrier or the attribute of analog adapt.
Owing to have the average particle size particle size that is lower than 10 μ m (0.5 to 10 μ m), described inorganic powder can be through surface treatment, as long as its attribute is not weakened, what use is organic acid, mineral acid, silane coupling agent, coupling agent based on titanate esters, based on the coupling agent of aluminium, surfactant, or other is used to prevent that secondary from assembling and the surface conditioning agent of promotion powder dispersiveness.Especially, surface treatment can be according to enforcement as described below: at first surface conditioning agent is dissolved in organic solvent or the water.In solution, add described inorganic powder then and stir the mixture.Then, solvent evaporated, residue in about 50 to 200 ℃ of heating above 2 hours.As selection, surface conditioning agent can add when photo-sensitive composition is formed lotion.
In the photosensitive insulative paste composition of the present invention, for total composition (=100 weight portion), organic component and inorganic powder ratio separately can be usually in 5 to 35 weight portions and 95 to 65 weight portion scopes, be preferably in 10 to 30 weight portions and 90 to the 70 weight portion scopes, more preferably in 15 to 25 weight portions and 85 to the 75 weight portion scopes.If the amount of organic component is lower than 5 weight portions, just can cause the photopolymerization deficiency.This will cause that image-region decomposes in the developing process, cause the imaging failure.Under comparing, if the amount of organic component more than 35 weight portions, the gained pattern just may break away from when oven dry.
Photosensitive insulative paste composition can prepare by dissolving or disperse the components in the solvent.The solvent of described purposes can be any solvent, as long as it has high-affinity for inorganic powder, can the excellent dissolution organic component, and can give described photosensitivity insulation composition with suitable viscosity, and be easy to evaporation and get final product.The particular instance of this solvent can comprise ketone, for example diethyl ketone, methyl butyl ketone, two acetone and cyclohexanone; Alcohols, for example n-amyl alcohol, 4-methyl-2-amylalcohol, cyclohexanol and diacetone alcohol; Ether alcohol class, for example glycol monomethyl methyl ether, ethylene glycol monomethyl ether, ethylene glycol monobutyl ether, propylene glycol monomethyl ether, propylene glycol list ethylether, diglycol monotertiary methyl ether, carbiphene, diethylene glycol dimethyl ether and diethylene glycol diethyl ether; Representative examples of saturated aliphatic monocarboxylic acid Arrcostab; For example n-butyl acetate and pentyl acetate; Lactic acid ester, for example ethyl lactate and n-butyl lactate; With the ether-ether class, for example methylcellosolve acetate, ethyl cellosolve acetate, propylene glycol monomethyl ether, propylene glycol list ethylether acetic acid esters, 3-ethoxyl ethyl propionate, acetate 2-methoxyl butyl ester, acetate 3-methoxyl butyl ester, acetate 4-methoxyl butyl ester, acetate 2-methyl-3-methoxyl butyl ester, acetate 3-methyl-3-methoxyl butyl ester, acetate 3-ethyl-3-methoxyl butyl ester, acetate 2-ethoxy butyl ester, acetate 4-ethoxy butyl ester, acetate 4-propoxyl group butyl ester and acetate 2-methoxyl pentyl ester.These solvents both can use individually, also can two or more mix use.
For the viscosity that makes photosensitive insulative paste composition remains on a good scope, total amount (=100 weight portion) for organic component and inorganic powder, used quantity of solvent is preferably 300 weight portions or lower, and more preferably 10 to 70 weight portions most preferably are 25 to 35 weight portions.
From the application of its expection, photosensitive insulative paste composition of the present invention both can be used as liquid state, also can be coated on base material by serigraphy or other various technology.In needing the process application of high precision, the barrier of PDPs for example, described composition is preferably used as photosensitive film.In this manner, the degree of accuracy of the pattern that forms can significantly promote, thereby can obtain having barrier or its analog of pinpoint accuracy.Described photosensitive film can form to supporting film by applying photosensitive insulative paste composition of the present invention, to obtain the film that thickness is 10 to 100 μ m.For example, can be the tough film that forms by synthetic resin of 15 to 125 μ m thickness, for example polyethylene terephthalate, tygon, polypropylene, polycarbonate and Polyvinylchloride as the supporting film of this purposes.If necessary, described supporting film can be handled with detackifier, makes film be easy to shift.Described composition can be used coater, bar coater, wired bar coater, roll coater, or curtain flow coater and being coated on the supporting film.Particularly roll coater can form even and thick film, thereby is preferred.Diaphragm can be coated on the photosensitive film, in order to protect described photosensitivity paste composition when the photosensitive film non-working condition.Diaphragm as this purposes can be silicone coating or the siloxane baked film that is about 15 to 125 μ m, by polyethylene terephthalate, and polypropylene, or tygon forms.
To describe with photosensitive insulative paste composition of the present invention subsequently and form required method of patterning.At first photosensitive insulative paste composition is coated on base material, forms rete with coating or transfer technique.With the activation ray, for example ultraviolet then, laser, X-ray, and electron beam see through mask and shine on the composition rete, and the picture of publishing picture exposes.Exposure back image develops in alkaline developer or water.Unexposed area will dissolve in developer, make and stay pattern on the base material.If necessary, can dry the rete of patterning.As selection, the whole surface of photosensitive insulative paste composition rete can not add covers and exposes.In this situation, can not carry out development step and form pattern.If necessary, base material can be dried subsequently.When needs formed high-precision patterns, photosensitive film at first was stripped from protective film, and photosensitive insulative paste composition is transferred to and forms rete on the base material.Described rete is being covered down or not exposure with covering, and it is being peeled off supporting film.The rete of covering down exposure develops to form pattern, and the rete of not covering exposure is handled without development step and hardened, and dries where necessary.Described base material can be a glass baseplate, has for example bus electrode (bus electrode) glass baseplate formed thereon, or ceramic base material.In shifting described photosensitive insulative paste composition rete process, use hot pressing that described composition rete and substrate surface are kept in touch, for example, use the hot rolling laminator.Implementing the hot pressing preferred pressure is 1 to 5kg/cm
2, and rolling speed is 0.1 to 10.0 meter/minute, the surface temperature of base material rises to 80 to 140 ℃.Described base material can be preheating to 40 to 100 ℃.The ray emitter of described paste composition of being used to expose can be the actinolyte that generally is used for photoetching, perhaps is used to produce the exposure sources of semiconductor and LCD (LCDs).
The basic component of the alkaline developer that uses can comprise alkaline metal in development step, for example the oxyhydroxide of lithium, sodium, potassium, carbonate, supercarbonate, phosphate and pyrophosphate; Primary amine compounds, for example benzylamine and butylamine; Secondary-amine compound, for example dimethylamine, dibenzylamine and diethanolamine; Tertiary amine compounds, for example trimethylamine, triethylamine and triethanolamine; Cyclic amine compound, for example morpholine, piperazine and pyridine; Polyamine compounds, for example ethylenediamine and hexane diamine; Ammonium hydroxide compounds, for example Tetramethylammonium hydroxide, tetraethyl ammonium hydroxide, trimethyl benzyl ammonium hydroxide and trimethylphenyl benzylic hydrogens amine-oxides; Hydroxide sulfonium compounds, for example trimethyl hydroxide sulfonium, diethylmethyl hydroxide sulfonium and dimethyl benzyl hydroxide sulfonium; Choline; With the damping fluid that contains silicate.Type, the concentration of composition and developer, same also free, temperature, mode of operation (as, soak, stir drip washing, spray, and stir), and the equipment that uses in the development step, these can do suitably to select according to the attribute of described photosensitive insulative paste composition.
Baking step can carry out any sufficiently high can burning under the temperature that is present in organic material in the described photosensitive insulative paste composition.For example, this step can be carried out 10 to 90 minutes at 400 ℃ to 600 ℃.
Photosensitive insulative paste composition of the present invention can be widely used in produces thick multilayer circuit, also can be used to produce plasma scope, plasma addressed liquid crystal display, with other various displays, be particularly suitable for the barrier that uses among the production high precision PDPs, especially, be suitable for producing the dielectric that uses among the PDPs.
Embodiment
Describe the present invention now with reference to several embodiment, these embodiment do not limit the present invention in any way.
Embodiment 1
(preparation of photosensitive insulative paste composition)
Following organic component was stirred 3 hours, mix, form solution (solid constituent=50%): the hydroxypropyl cellulose of 15 weight portions is as water-soluble cellulose derivative, styrene/methacrylic acid hydroxyl ethyl ester multipolymer (the styrene/methacrylic acid hydroxyl ethyl ester=55/45 (weight %) of 33 weight portions, molecular weight=8500) as the acryl resin of hydroxyl, the 2-hydroxyl of 39 weight portions-3-phenoxy propyl acrylate (ProductName: M-600A, Kyoeisha chemicals company limited) as photo polymerization monomer, 1.0 2 of weight portion, 2-dimethoxy-2-phenyl acetophenone (ProductName: IR-651, Ciba Geigy company limited) as Photoepolymerizationinitiater initiater, the dicyclohexyl phthalate of 12 weight portions as the 3-methoxyl-3-methyl butanol of plastifier and 100 weight portions as solvent.This solution (solid constituent=50%) of 35 weight portions is mixed/kneads with glass dust as 82.5 weight portions of inorganic powder, form photosensitive insulative paste composition.
(preparation of photosensitive film)
The photosensitive insulative paste composition that will obtain like this with flanging coater (lip coater) is coated to the polyethylene terephthalate supporting film.100 ℃ of dry coatings 6 minutes to remove solvent fully.Stay the photosensitive insulative paste film on the supporting film of being formed at of thick 27 μ m.Again the photosensitive insulative paste coating is covered polyethylene film with thick 25 μ m.Promptly finish the photosensitive film preparation.
(evaluation of photosensitive film)
Use is set in 105 ℃ the laminated device of hot rolling, and glass baseplate is preheating to 80 ℃, peels off the polyethylene film while on the gained photosensitive film, and itself and glass baseplate is laminated.The air pressure and the laminate speed that adopt are respectively 3kg/cm
2With 1.0 meters/minute.Then peel off the polyethylene terephthalate supporting film.As light source, ultraviolet ray is promptly with 500mJ/cm with extra-high-pressure mercury vapour lamp
3Dosage expose on the photosensitivity coating by mask with square test pattern.For the described pattern that develops, with 30 ℃ water with 3kg/cm
2Pressure, be injected on the exposure coating, through a time cycle, five times in this way, as long as rete no show breakpoint.Term used herein " breakpoint " refers to the time that the material in the unexposed area is removed fully.
The minimum feature that keeps is decided to be the bounding force standard of measurement of the pattern that forms, and is defined as 40 μ m.Form pattern with sweep electron microscope observation station, find that it is a trapezoidal pattern.Dry the pattern that this mode forms, to estimate its shape stability.Baking step at first is to heat described film with 1.0 ℃/minute speed, keeps 30 minutes at 580 ℃ then.The pattern of drying is proved to be gratifying.
Comparing embodiment 1
(preparation of photosensitive insulative paste composition)
Following organic component was stirred 3 hours, mix, form solution: the hydroxypropyl cellulose of 15 weight portions is as water-soluble cellulose derivative, styrene/methacrylic acid hydroxyl ethyl ester multipolymer (the styrene/methacrylic acid hydroxyl ethyl ester=55/45 (weight %) of 33 weight portions, molecular weight=25000) as the acryl resin of hydroxyl, the 2-hydroxyl of 39 weight portions-3-phenoxy propyl acrylate (ProductName: M-600A, Kyoeisha chemicals company limited) as photo polymerization monomer, 1.0 2 of weight portion, 2-dimethoxy-2-phenyl acetophenone (ProductName: IR-651, Ciba Geigy company limited) as Photoepolymerizationinitiater initiater, the dicyclohexyl phthalate of 12 weight portions as the 3-methoxyl-3-methyl butanol of plastifier and 100 weight portions as solvent.This solution of 35 weight portions and the glass dust as 82.5 weight portions of inorganic powder are kneaded, formed photosensitive insulative paste composition.
(preparation of photosensitive film)
The photosensitive insulative paste composition that will obtain like this with flanging coater (lip coater) is coated to the polyethylene terephthalate supporting film.100 ℃ of dry coatings 6 minutes to remove solvent fully.Stay the photosensitive insulative paste film on the supporting film of being formed at of thick 27 μ m.Again the photosensitive insulative paste coating is covered polyethylene film with thick 25 μ m.Promptly finish the photosensitive film preparation.
(evaluation of photosensitive film)
Use is set in 105 ℃ the laminated device of hot rolling, and glass baseplate is preheating to 80 ℃, peels off the polyethylene film while on the gained photosensitive film, and itself and glass baseplate is laminated.The air pressure and the laminate speed that adopt are respectively 3kg/cm
2With 1.0 meters/minute.Then peel off the polyethylene terephthalate supporting film.As light source, ultraviolet ray is promptly with 500mJ/cm with extra-high-pressure mercury vapour lamp
3Dosage expose on the photosensitivity coating by mask with square test pattern.For the described pattern that develops, with 30 ℃ water with 3kg/cm
2Pressure, be injected on the exposure coating, through a time cycle, five times in this way, as long as rete no show breakpoint.
The minimum feature that keeps is decided to be the bounding force standard of measurement of the pattern that forms, and is defined as 40 μ m.The development of described pattern is incomplete, can see residue.
Industrial applicibility
As previously proposed, photosensitive insulative paste composition of the present invention contains organic component, and described organic component makes composition have higher developer repellence, and it is suitable for forming thick and the rete of height sensitization still, thereby can form high-precision patterns. Photosensitive insulative paste composition of the present invention is suitable for producing photosensitive film.
Claims (6)
1. photosensitive insulative paste composition, comprise a kind of organic component and a kind of inorganic powder, wherein said organic component comprises (A) water-soluble cellulose derivative, (B) molecular weight of hydroxyl is 20000 or lower acryl resin, (C) photo polymerization monomer and (D) Photoepolymerizationinitiater initiater.
2. photosensitive insulative paste composition according to claim 1, for the component A and the B component total amount of 100 weight portions in the organic component, described composition contains the B component of the component A and 90 to 50 weight portions of 10 to 50 weight portions.
3. photosensitive insulative paste composition according to claim 1, wherein inorganic powder is a glass powder.
4. photosensitive insulative paste composition according to claim 1, for the component A and the component C total amount of 100 weight portions in the organic component, described composition contains the component A of 10 to 50 weight portions and the component C of 90 to 50 weight portions.
5. photosensitive insulative paste composition according to claim 1, for the organic component and the inorganic powder total amount of 100 weight portions, described composition contains the organic component of 5 to 35 weight portions and the inorganic powder of 95 to 65 weight portions.
6. photosensitive film comprises supporting film and is formed on the supporting film rete that any one photosensitive insulative paste composition by claim 1 to 5 forms.
Applications Claiming Priority (3)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2004082416A JP4282518B2 (en) | 2004-03-22 | 2004-03-22 | Photosensitive insulating paste composition and photosensitive film using the same |
| JP082416/2004 | 2004-03-22 | ||
| PCT/JP2005/004888 WO2005091071A1 (en) | 2004-03-22 | 2005-03-14 | Photosensitive insulative paste composition and photosensitive film using the same |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1934496A CN1934496A (en) | 2007-03-21 |
| CN1934496B true CN1934496B (en) | 2010-10-20 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN200580009109.0A Expired - Fee Related CN1934496B (en) | 2004-03-22 | 2005-03-14 | Photosensitive insulative paste composition and photosensitive film using the same |
Country Status (5)
| Country | Link |
|---|---|
| JP (1) | JP4282518B2 (en) |
| KR (1) | KR100868550B1 (en) |
| CN (1) | CN1934496B (en) |
| TW (1) | TWI311688B (en) |
| WO (1) | WO2005091071A1 (en) |
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| KR100754485B1 (en) * | 2005-12-14 | 2007-09-03 | 엘지전자 주식회사 | A dielectric layer manufacturing method of plasma display panel |
| US8158218B2 (en) * | 2008-05-02 | 2012-04-17 | Konica Minolta Opto, Inc. | Process for producing optical film, optical film, polarizer, and liquid crystal display |
| CN106773533A (en) * | 2017-02-09 | 2017-05-31 | 中国科学院上海微系统与信息技术研究所 | A kind of photoresist and its application process |
| CN113039628A (en) | 2018-11-15 | 2021-06-25 | 东京应化工业株式会社 | Protective film forming agent for plasma dicing and method for manufacturing semiconductor chip |
| CN112500156B (en) * | 2020-12-08 | 2022-06-03 | 北京科技大学 | Blue zirconia ceramic and preparation method thereof |
| CN115185160B (en) * | 2022-09-09 | 2023-06-27 | 之江实验室 | Laser direct-writing photoresist composition based on cellulose derivative and patterning method |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1324091A (en) * | 2000-02-22 | 2001-11-28 | 三菱重工业株式会社 | Composite material used for mfg. isolation sheet of thin layer display panel |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP1387384A1 (en) * | 1996-01-22 | 2004-02-04 | Hitachi Chemical Co., Ltd. | Phosphor pattern, processes for preparing the same and photosensitive element to be used for the same |
| KR100327360B1 (en) * | 1999-04-22 | 2002-03-06 | 구자홍 | Photosensitive paste composition with low temperature firing property for plasma display panel |
| KR100663100B1 (en) * | 2000-09-01 | 2007-01-02 | 후지 휘루무오린 가부시키가이샤 | Photosensitive Composition, Photosensitive Coated Substance, and Fine-pattern Structure |
| JP3827196B2 (en) * | 2001-05-01 | 2006-09-27 | 東京応化工業株式会社 | Photosensitive insulating paste composition and photosensitive film using the same |
| JP4130102B2 (en) * | 2001-09-18 | 2008-08-06 | 富士フイルム株式会社 | Radiation sensitive coloring composition |
-
2004
- 2004-03-22 JP JP2004082416A patent/JP4282518B2/en not_active Expired - Lifetime
-
2005
- 2005-03-14 KR KR1020067019360A patent/KR100868550B1/en active IP Right Grant
- 2005-03-14 WO PCT/JP2005/004888 patent/WO2005091071A1/en active Application Filing
- 2005-03-14 CN CN200580009109.0A patent/CN1934496B/en not_active Expired - Fee Related
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1324091A (en) * | 2000-02-22 | 2001-11-28 | 三菱重工业株式会社 | Composite material used for mfg. isolation sheet of thin layer display panel |
Non-Patent Citations (3)
| Title |
|---|
| JP特开2002-311582A 2002.10.23 |
| JP特开2002-82428A 2002.03.22 |
| JP特开2004-69755A 2004.03.04 |
Also Published As
| Publication number | Publication date |
|---|---|
| WO2005091071A1 (en) | 2005-09-29 |
| JP4282518B2 (en) | 2009-06-24 |
| KR20070007107A (en) | 2007-01-12 |
| TW200602807A (en) | 2006-01-16 |
| KR100868550B1 (en) | 2008-11-13 |
| TWI311688B (en) | 2009-07-01 |
| CN1934496A (en) | 2007-03-21 |
| JP2005266663A (en) | 2005-09-29 |
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