CN100461328C - Inorganic particle containing composition for plasma display panel, transfer film and process for producing plasma display panel - Google Patents

Inorganic particle containing composition for plasma display panel, transfer film and process for producing plasma display panel Download PDF

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Publication number
CN100461328C
CN100461328C CNB2004800109193A CN200480010919A CN100461328C CN 100461328 C CN100461328 C CN 100461328C CN B2004800109193 A CNB2004800109193 A CN B2004800109193A CN 200480010919 A CN200480010919 A CN 200480010919A CN 100461328 C CN100461328 C CN 100461328C
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material layer
formation material
film formation
film
methyl
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CN1777970A (en
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川岸诚治
山下隆德
伊藤克美
井上靖健
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JSR Corp
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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
    • H01J11/44—Optical arrangements or shielding arrangements, e.g. filters, black matrices, light reflecting means or electromagnetic shielding means
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C3/00—Glass compositions
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00—Use of inorganic substances as compounding ingredients
    • C08K3/01—Use of inorganic substances as compounding ingredients characterized by their specific function
    • G—PHYSICS
    • G02—OPTICS
    • G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
    • G02B5/00—Optical elements other than lenses
    • G02B5/20—Filters
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J2211/00—Plasma display panels with alternate current induction of the discharge, e.g. AC-PDPs
    • H01J2211/20—Constructional details
    • H01J2211/22—Electrodes
    • H01J2211/225—Material of electrodes
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J2211/00—Plasma display panels with alternate current induction of the discharge, e.g. AC-PDPs
    • H01J2211/20—Constructional details
    • H01J2211/34—Vessels, containers or parts thereof, e.g. substrates
    • H01J2211/36—Spacers, barriers, ribs, partitions or the like

Abstract

The present invention provides a composition containing inorganic particles for use in a plasma display panel; a transfer film from the composition; and a process for producing a plasma display panel. The composition comprises inorganic particles [A] and polymer [B] having repeating units of the formula (I). The composition may further comprise a plasticizer and/or a silane coupling agent. A transfer film having various excellent properties can be produced from the composition. Plasma display panel constituent elements excelling in various properties can be efficiently formed in a low temperature/short time firing step according to the process for producing a plasma display panel. The process is characterized in, for example, that it includes a step of forming a dielectric layer on a substrate by transferring a film forming material layer obtained from the composition onto the substrate and firing the transferred film forming material layer.

Description

The manufacture method of inorganic particle containing composition for plasma display panel, transfer film and Plasmia indicating panel
Technical field
The present invention relates to the manufacture method of a kind of inorganic particle containing composition for plasma display panel, transfer film and Plasmia indicating panel.
Background technology
In recent years, show body as flat fluorescence, plasma display just is being subjected to gazing at of people.Fig. 1 is the cross sectional shape of the Plasmia indicating panel (below be also referred to as " PDP ") of expression AC type.In the figure, 1 and 2 is glass substrates of antagonism configuration, the 3rd, and the next door forms the unit by glass substrate 1, glass substrate 2 and next door 3 subregions.The 4th, be fixed in the transparency electrode of glass substrate 1; the 5th, with the resistance that reduces transparency electrode 4 be purpose, the bus electrode that on this transparency electrode 4, forms; the 6th, be fixed in the address electrode of glass substrate 2; the 7th, be maintained at the fluorescent material in the unit; the 8th, the dielectric layer that on the surface of the glass substrate 1 that is used for covering transparent electrode 4 and bus electrode 5, forms; the 9th, the dielectric layer that on the surface of the glass substrate 2 that is used for overlay address electrode 6, forms, the 10th, the diaphragm that constitutes by magnesium oxide for example.In addition, for color PDP,, between glass substrate and dielectric layer, be provided with colour filter (color filter) (red, green or blue) or black matrix etc. in order to obtain the high image of contrast.
Manufacture method as such PDP dielectric, next door, electrode, fluorophor, colour filter and black streaking (matrix), the preferred use, on substrate, form and contain photosensitive inorganic particle resin bed, on this film by the basis of photomask irradiation ultraviolet radiation on by developing, remaining pattern on substrate is with its photoetching process of burning till etc.
Above-mentioned photoetching process pattern precision on principle is outstanding, particularly in the method for using transfer film, can form the homogeneity of thickness and the outstanding pattern of homogeneity on surface.But, in the operation of burning till the film formation material layer, if set at high temperature long firing condition, fully carry out the fusion of film formation material layer, in the film formation material layer, be easy to generate the crack, in addition, set at high temperature for a long time firing condition to bringing firing furnace very big burden, and productivity ratio is low.So need the film formation material layer at low temperature, firing process in the short time.
Summary of the invention
The present invention is based on aforesaid situation and carries out.
What the 1st purpose of the present invention was to be provided at the inscape (for example next door, electrode, resistive element, dielectric layer, fluorophor, colour filter or black matrix) that can form the outstanding PDP of surface smoothing in the firing process in low temperature, short time aptly contains the inorganic particulate composition.
What the 2nd purpose of the present invention was to provide the outstanding transfer film of the pliability that can make the film formation material layer contains the inorganic particulate composition.
What the 3rd purpose of the present invention was to provide the outstanding transfer film of the transfer printing that can make the film formation material layer (the heating adhesiveness of substrate relatively) contains the inorganic particulate composition.
The 4th purpose of the present invention is to be provided at the transfer film that can form the inscape of the outstanding PDP of surface smoothing in the firing process in low temperature and short time effectively.
The 5th purpose of the present invention is to provide the outstanding transfer film of pliability of film formation material layer.
The 6th purpose of the present invention is to provide the outstanding transfer film of pliability (the heating adhesiveness of substrate relatively) of film formation material layer.
The 7th purpose of the present invention is to be provided at the PDP manufacture method that can form the inscape of the outstanding PDP of surface smoothing in the firing process in low temperature and short time effectively.
The 8th purpose of the present invention is to be provided at the PDP manufacture method that can form the big dielectric layer of thickness in the firing process in low temperature and short time effectively.
The 9th purpose of the present invention is to be provided at the PDP manufacture method that can form the dielectric layer that large-scale panel needs in the firing process in low temperature and short time effectively.
The 10th purpose of the present invention is to be provided at the PDP manufacture method of the outstanding dielectric layer of the homogeneity that has thickness in the firing process in low temperature and short time.
The 11st purpose of the present invention is to be provided at the PDP manufacture method that has the outstanding dielectric layer of surface smoothing in the firing process in low temperature and short time.
Of the present inventionly contain the binding resin that the inorganic particulate composition contains the polymer that [A] inorganic particulate and containing has the repetitive that [B] represent with following formula (1) (below be also referred to as " polymer [B-1] ").Like this, inorganic particulate is strong to the absorption of adhering resin, shortens by make the distance between inorganic particulate when burning till, and makes burning till in low temperature, short time become possibility.
Figure C200480010919D00071
(in the formula, X represents hydrogen atom or methyl, R 1Alkylene, the n of expression singly-bound, methylene or carbon number 2～5 represent 1～6 integer.)
The inorganic particulate composition that contains of the present invention also can be the composition that further contains [C] radioactivity-sensitive composition (below be also referred to as " radioactivity-sensitive contains the inorganic particulate composition ").
Transfer film of the present invention has by above-mentioned and contains the film formation material layer that the inorganic particulate composition obtains.
The manufacture method of 1PDP of the present invention (below be also referred to as " manufacture method of PDP (1) ") has following operation: will be contained the film formation material layer that the inorganic particulate composition obtains and be transferred on the substrate by of the present invention, by burning till the film formation material layer of transfer printing, on aforesaid substrate, form dielectric layer.
The manufacture method of 2PDP of the present invention (below be also referred to as " manufacture method of PDP (2) ") has following operation: will be contained the film formation material layer that the inorganic particulate composition obtains and be transferred on the substrate by of the present invention, on the film formation material layer of transfer printing, form etchant resist, this etchant resist of exposure-processed, form the sub-image of resist pattern, this etchant resist of development treatment, make the resist patterned surfacesization, this film formation material layer of etch processes, form the patterned layer corresponding with the resist pattern, handle this patterned layer by burning till, form from the next door, electrode, resistive element, dielectric layer, fluorophor, the inscape of selecting in colour filter and the black matrix.
In addition, the manufacture method of 3PDP of the present invention (below be also referred to as " manufacture method of PDP (3) ") has following operation: on support film, form etchant resist with by the stacked film that contains the film formation material layer that the inorganic particulate composition obtains of the present invention, to be transferred on the substrate at the stacked film that forms on the support film, exposure-processed constitutes the etchant resist of this stacked film, form the sub-image of resist pattern, this etchant resist of development treatment, make the resist patterned surfacesization, this film formation material layer of etch processes, form the patterned layer corresponding with the resist pattern, handle this patterned layer by burning till, form from the next door, electrode, resistive element, dielectric layer, fluorophor, the inscape of selecting in colour filter and the black matrix.
The manufacture method of 4PDP of the present invention (below be also referred to as " manufacture method of PDP (4) ") has following operation: will be contained the film formation material layer that radiation inorganic particulate composition obtains and be transferred on the substrate by of the present invention, this film formation material layer of exposure-processed, form the sub-image of pattern, this film formation material layer of development treatment, form patterned layer, handle this patterned layer by burning till, form the inscape of from next door, electrode, resistive element, dielectric layer, fluorophor, colour filter and black matrix, selecting.
Description of drawings
Fig. 1 is the schematic diagram of the cross sectional shape of expression AC type plasma displaying panel.
Fig. 2 A is the fragmentary cross sectional view of expression transfer film of the present invention, and Fig. 2 B is the sectional view that the layer of this transfer film of expression constitutes.
Fig. 3 A-3E is the fragmentary cross sectional view of an example of the formation operation (the formation operation and the exposure process of transfer printing process, etchant resist) in the next door of expression in the manufacture method of the present invention.
Fig. 4 A-4D is the fragmentary cross sectional view of an example of the formation operation (developing procedure, etching work procedure and firing process) in the next door of expression in the manufacture method of the present invention.
Among the figure, 1-glass substrate, 2-glass substrate; 3-next door, 4-transparency electrode, 5-bus electrode; 6-address electrode, 7-fluorescent material, 8-dielectric layer; 9-dielectric layer, 10-protective layer, F1-support film; F2-film formation material layer, F3-cover film, 11-glass substrate; 12-electrode, 13-dielectric layer, 20-transfer film; 21-film formation material layer, 22-support film, 25-partition pattern layer; the residual portion of 25A-material layer, 25B-material layer removal portion, 31-etchant resist; 35-resist pattern; the residual portion of 35A-resist, 35B-resist removal portion, 40-next door; 50-panel material; M-exposure mask, MA-transmittance section, MB-light shielding part.
Embodiment
Below to the inorganic particulate composition (following also can be called " composition " is elaborated) that contains of the present invention.
Composition of the present invention contains inorganic particulate, binding resin and solvent usually.In binding resin, contain polymer [B-1].
＜inorganic particulate 〉
Inorganic substances to the inorganic particulate that constitutes composition of the present invention are not particularly limited, can be according to the purposes (kind of the inscape of PDP) of the sintered body that forms by said composition suitable the selection.
For the inorganic particulate that in the composition that is used to form " dielectric layer " or " next door " that constitute PDP, contains, can enumerate the glass powder of softening point in the scope of 350～700 ℃ (being preferably 400～600 ℃) here.At the softening point of glass powder during less than 350 ℃, in the firing process of the film formation material layer that utilizes said composition, organic substance at binding resin etc. is decomposed the stage of removing fully, glass powder will fusion, so part of residual organic matter matter in the dielectric layer that forms, dielectric layer is painted as a result, and its light transmittance reduces.On the other hand, when glass powder divides softening point to surpass 700 ℃, because need be with burning till than 700 ℃ of high high temperature, so on glass substrate, deform easily etc.
Object lesson as suitable glass powder can be illustrated as (1) lead oxide, boron oxide and silica (PbO-B 2O 3-SiO 2System) mixture, (2) lead oxide, boron oxide, silica and magnesium oxide (PbO-B 2O 3-SiO 2-MgO system) mixture, (3) lead oxide, boron oxide, silica and aluminium oxide (PbO-B 2O 3-SiO 2-Al 2O 3System) mixture, (4) lead oxide, boron oxide, silica and calcium oxide (PbO-B 2O 3-SiO 2-CaO system) mixture, (5) lead oxide, zinc oxide, boron oxide and silica (PbO-ZnO-B 2O 3-SiO 2System) mixture etc.
These glass powders also can contain (and using) in the composition of the inscape (for example electrode, resistive element, fluorophor, colour filter or black matrix) beyond being used to form dielectric layer and next door.In the content of the frit that contains the inorganic particulate resin combination that is used for obtaining these panel materials full dose with respect to inorganic particulate, be generally below the 90 weight %, be preferably 50～90 weight %.
As the inorganic particulate that in the composition that is used to form " electrode " that constitute PDP, contains, can enumerate the metallic that constitutes by Ag, Au, Al, Ni, Ag-Pd alloy, Cu, Cr etc.
In being used to form the composition of dielectric layer, also can contain these metallics with form with glass powder and usefulness.The content that the metallic in the composition is used in dielectric layer formation is generally 10 weight % with respect to the inorganic particulate full dose, is preferably 0.1～5 weight.
As the inorganic particulate that in the composition that is used to form " resistive element " that constitute PDP, contains, can enumerate by RuO 2On the particle that constitutes.
As the inorganic particulate that in the composition that is used to form " fluorophor " that constitute PDP, contains, can enumerate by Y 2O 3: Eu 3+, Y 2SiO 5: Eu 3+, Y 3Al 5O 12: Eu 3+, YVO 4: Eu 3+, (Y, Gd) BO 3: Eu 3+, Zn 3(PO 4) 2: the redness fluorescent material of Mn etc.; Zn 2SiO 4: Mn, BaAl 12O 19: Mn, BaMgAl 14O 23: Mn, LaPO 4: (Ce, Tb), Y3 (Al, Ga) 5O 12: the green fluorescent material of Tb etc.; Y 2SiO 5: Ce, BaMgAl 10O 17: Eu 2+, BaMgAl 14O 23: Eu 2+, (Ca, Sr, Ba) 10(PO 4) 6C 12: Eu 2+, (Zn, Cd) particle that constitutes with fluorescent material etc. of the blueness of S:Ag etc.
As the inorganic particulate that in the composition that is used to form " colour filter " that constitute PDP, contains, can enumerate by Fe 2O 3, Pb 3O 4Deng the redness material; Cr 2O 3Deng the green material; 2 (Al 2Na 2Si 3O 10) Na 2S 4Deng the particle that constitutes with material etc. of blueness.
As the inorganic particulate that in the composition that is used to form " the black matrix " that constitute PDP, contains, can enumerate the particle that constitutes by Mn, Fe, Cr etc.
＜binding resin 〉
The binding resin that constitutes composition of the present invention is for containing the resin of polymer [B-1].Binding resin can be separately a polymer [B-1], also can for other mixture of polymers.As other polymer, be suitable for above-mentioned polymer [B-1] acrylic resin in addition.
Polymer [B-1] is preferably acrylic resin for having the polymer with the repetitive of above-mentioned formula (1) expression.By containing acrylic resin as binding resin, performance (heating) adhesiveness outstanding in the film formation material layer that forms with respect to substrate.Thereby when coating composition of the present invention was made transfer film on support film, the transfer film that obtains became the outstanding film of transfer printing (to the adhesiveness that enters of substrate) of film formation material layer.
As the acrylic resin (polymer [B-1] and other polymer) that constitutes composition of the present invention, can have the adhesiveness of appropriateness and make inorganic particulate bonding, from the selection the polymer (condensation polymer) that processings (400～600 ℃) removed by complete oxidation of burning till by film formation material.
Repetitive with above-mentioned formula (I) expression utilizes monomer (being total to) polymerization of following formula (i) expression to form by making.
Figure C200480010919D00101
(in the formula, X, R 1Identical with the definition of n with above-mentioned formula (I).)
In above-mentioned formula (i), as R 1, preferred especially singly-bound or methylene.In addition, as n, preferred especially 1.
Object lesson as the monomer of representing with above-mentioned formula (i); can enumerate glycidol (methyl) acrylate, β-methyl glycidol (methyl) acrylate, (methyl) third rare acyl group methyl cyclohexane olefinic oxide, 3,4-ethoxy cyclohexyl (methyl) methyl acrylate etc.
Polymer [B-1] is preferably with the monomer of above-mentioned formula (i) expression and the copolymer of other monomer, as other monomer, is preferably other (methyl) acrylate compounds.
As this other the object lesson of (methyl) acrylate compounds, can enumerate (methyl) methyl acrylate, (methyl) ethyl acrylate, (methyl) propyl acrylate, (methyl) isopropyl acrylate, (methyl) butyl acrylate, (methyl) isobutyl acrylate, (methyl) tert-butyl acrylate, (methyl) acrylic acid pentyl ester, (methyl) acrylic acid pentyl ester, (methyl) acrylic acid isopentyl ester, (methyl) Hexyl 2-propenoate, (methyl) acrylic acid heptyl ester, (methyl) 2-ethyl hexyl acrylate, (methyl) Isooctyl acrylate monomer, ethyl (methyl) Hexyl 2-propenoate, (methyl) acrylic acid ester in the ninth of the ten Heavenly Stems, (methyl) decyl acrylate, (methyl) isodecyl acrylate, (methyl) acrylic acid undecyl ester, (methyl) dodecylacrylate, (methyl) lauryl acrylate, (methyl) acrylic acid stearyl, (methyl) alkyl acrylates such as (methyl) acrylic acid isooctadecane base ester;
(methyl) acrylic acid hydroxy alkyl esters such as (methyl) acrylic acid hydroxyl methyl esters, (methyl) acrylic acid 2-hydroxypropyl acrylate, (methyl) acrylic acid 3-hydroxypropyl acrylate, (methyl) acrylic acid 2-hydroxy butyl ester, (methyl) acrylic acid 3-hydroxy butyl ester, (methyl) acrylic acid 4-hydroxy butyl ester;
(methyl) phenoxyethyl acrylate, (methyl) acrylic acid 2-hydroxyl-(methyl) acrylic acid benzene oxyalkyl esters such as 3-benzene oxygen propyl ester; (methyl) alkoxyalkyl acrylates such as (methyl) acrylic acid 2-methoxy ethyl ester, (methyl) acrylic acid 2-ethoxy ethyl ester, (methyl) acrylic acid 2-the third 2-ethoxyethyl acetate, (methyl) acrylic acid 2-fourth 2-ethoxyethyl acetate, (methyl) acrylic acid 2-methoxy butyl ester;
The poly-alkylene glycols esters of (methyl) acrylic acid such as single (methyl) polyalkylene glycol acrylate ester, (methyl) acrylic acid ethoxy binaryglycol ester, (methyl) acrylic acid methoxy macrogol ester, (methyl) acrylic acid benzene oxygen macrogol ester, (methyl) acrylic acid nonyl benzene oxygen macrogol ester, (methyl) acrylic acid polypropylene glycol ester, (methyl) acrylic acid methoxy polypropylene glycol ester, (methyl) acrylic acid ethoxy polypropylene glycol ester, (methyl) acrylic acid nonyl benzene oxygen polypropylene glycol ester;
(methyl) acrylic acid cycloalkyl esters such as (methyl) cyclohexyl acrylate, (methyl) acrylic acid 4-butyl cyclohexyl, (methyl) acrylic acid two ring pentyl esters, (methyl) acrylic acid dicyclopentenyl ester, (methyl) acrylic acid dicyclopentadienyl ester, (methyl) acrylic acid norbornene ester, (methyl) isobornyl acrylate, (methyl) acrylic acid three ring esters in the last of the ten Heavenly stems;
(methyl) acrylic acid benzyl ester, (methyl) acrylic acid tetrahydro furfuryl ester etc.These (methyl) acrylate compounds can use separately, also can mix more than 2 kinds and use.
Wherein, preferably (methyl) alkyl acrylate, (methyl) acrylic acid hydroxy alkyl ester and (methyl) alkoxyalkyl acrylate, as particularly preferred (methyl) acrylate compounds, can enumerate (methyl) butyl acrylate, (methyl) EHA, (methyl) lauryl acrylate, (methyl) isodecyl acrylate, (methyl) acrylic acid 2-ethoxy ethyl ester and (methyl) acrylic acid 2-hydroxypropyl acrylate.
As other monomer beyond (methyl) acrylate compounds, so long as can with the compound of above-mentioned (methyl) acrylate compounds copolymerization, then be not particularly limited, for example can enumerate unsaturated carboxylic acid classes such as (methyl) acrylate, vinyl benzoic acid, maleic acid, vinyl benzene dioctyl phthalate; Vinyl benzyl methyl ether, vinyl glycidyl ether, styrene, α-methyl styrene, butadiene, isoprene etc. contain the vinyl free-radical polymerised compound.
In addition, in the formation of the inscape of the PDP that has utilized photoresist method described later, in the etch processes of film formation material layer, during essential alkali-soluble,, preferably contain carboxylic monomer as above-mentioned other co-polymerized monomer (combined polymerization composition).As the above-mentioned object lesson that contains carboxylic monomer, can enumerate acrylic acid, methacrylic acid, maleic acid, fumaric acid, citric acid, itaconic acid, citraconic acid, mesaconic acid, cinnamic acid, mono succinate (2-(methyl) third rare acyloxy ethyl), ω-carboxyl-polycaprolactam list (methyl) acrylate etc.Wherein, preferable methyl acrylic acid.
As the object lesson of preferred alkali soluble resin, for example can enumerate (methyl) acrylic resin, hydroxy styrenes resin, novolac resin, mylar etc. here.
In such alkali soluble resin, as preferred substance, can select the above-mentioned copolymer that contains between carboxylic monomer and (methyl) alkyl acrylate, (methyl) acrylic acid hydroxy alkyl ester and (methyl) alkoxyalkyl acrylate, as preferred (methyl) acrylate compounds, can enumerate (methyl) butyl acrylate, (methyl) EHA, (methyl) lauryl acrylate, (methyl) isodecyl acrylate, (methyl) acrylic acid 2-ethoxy ethyl ester and (methyl) acrylic acid 2-hydroxypropyl acrylate.
In polymer [B-1], with the usage ratio of the monomer of above-mentioned formula (i) expression with respect to whole monomer 100 weight portions (?), be generally 0.1～50 weight portion, be preferably 0.1～10 weight portion, more preferably 1～5 weight portion.
As the molecular weight of polymer [B-1], as the weight average molecular weight of the polystyrene conversion by gel permeation chromatography (hereinafter referred to as " GPC ") (following also be called simply " weight average molecular weight), be preferably 4; 000～300,000, more preferably 10; 000～200,000.
In addition, as also mixing other polymer that uses, the polymer that contains above-mentioned other (methyl) acrylate compounds can be enumerated as preferred polymers with polymer [B-1].
The ratio of the repetitive of representing with above-mentioned formula (1) in binding resin integral body is generally 0.1～50 weight %, is preferably 0.1～10 weight %, more preferably 1～5 weight %.And then the ratio that derives from the repetitive (comprising the repetitive with above-mentioned formula (1) expression) of (methyl) acrylate in binding resin integral body is preferably more than the 70 weight %, more preferably more than the 90 weight %.
Proportional as containing of the binding resin in the composition of the present invention, with respect to inorganic particulate 100 weight portions, be preferably 5～80 weight portions, more preferably 5～30 weight portions.In the ratio of binding resin during less than 5 weight portions, the maintenance inorganic particulate that can not bond reliably, in addition-aspect, when this ratio surpasses 80 weight portions, firing process needs for a long time, and perhaps the sintered body of Xing Chenging (for example dielectric layer) does not become and has full intensity or thickness material.
＜solvent 〉
Usually contain solvent in the composition of the present invention.As above-mentioned solvent,, can give the viscosity of appropriateness to the composition that obtains, by making its drying solvent of evaporative removal easily preferably with the compatibility of inorganic particulate, the favorable solubility of binding resin.
As the object lesson of this solvent, can the illustration diethyl ketone, ketone such as methyl butyl ketone, two acetone, cyclohexanone; Alcohols such as n-amyl alcohol, 4-methyl-2-amylalcohol, cyclohexanol, diacetone alcohol; Ethers such as glycol monoethyl ether, ethylene glycol monoethyl ether, ethylene glycol monobutyl ether, propylene glycol monomethyl ether, dihydroxypropane single-ether are alcohols; Unsaturated aliphatic such as n-butyl acetate, pentyl acetate monocarboxylic acid alkyl ether; Lactic acid ester such as ethyl lactate, n-butyl lactate; Methyl glycol acetate, ethyl cellosolve acetate, propylene glycol monomethyl ether acetate, ethyl-ethers such as 3-ethoxy-c acid esters are ester class etc.They can use more than 2 kinds alone or in combination.
Proportional as containing of the solvent in the composition of the present invention, maintain viewpoint the suitable scope from viscosity with composition, with respect to inorganic particulate 100 weight portions, be preferably below 40 weight portions, more preferably 5～30 weight portions.
＜dispersant 〉
Preferably in composition of the present invention, contain dispersant.As this dispersant, preferably use the silane coupling agent [containing saturated alkyl (alkyl) alkoxy silane] of following formula (2) expression.
(in the formula, p is 3～20 integer, and m is 1～3 integer, and n is 1～3 integer, and then a is the integer from 1～3.)
In with above-mentioned formula (2), the p of the carbon number of expression saturated alkyl is 3～20 integer, is preferably 4～16 integer.
Even make its contain p less than 3 contain saturated alkyl (alkyl) alkoxy silane, in the film formation material layer that obtains, also can not show sufficient pliability sometimes.On the other hand, p surpasses 20 the decomposition temperature height that contains saturated alkyl (alkyl) alkoxy silane, in the firing process of the film formation material layer that obtains, owing to do not decomposing the stage of removing organic substance (above-mentioned silane derivative) fully, glass powder meeting fusion, so the part of residual organic matter matter in the dielectric layer that forms, consequently the light transmittance of dielectric layer can reduce sometimes.
Object lesson as the silane coupling agent of representing with above-mentioned formula (2), can enumerate saturated alkyl dimethyl methyl TMOS class (a=1 such as n-pro-pyl dimethyl methyl TMOS, normal-butyl dimethyl methyl TMOS, positive decyl dimethyl methyl TMOS, n-hexadecyl dimethyl methyl TMOS, n-eicosane base dimethyl methyl TMOS, m=1, n=1);
Saturated alkyl diethyl methoxy silane class (a=1 such as n-pro-pyl diethyl methoxy silane, normal-butyl diethyl methoxy silane, positive decyl diethyl methoxy silane, n-hexadecyl diethyl methoxy silane, n-eicosane base diethyl methoxy silane, m=1, n=2);
Saturated alkyl dipropyl methoxy silane classes such as normal-butyl dipropyl methoxy silane, positive decyl dipropyl methoxy silane, n-hexadecyl dipropyl methoxy silane, n-eicosane base dipropyl methoxy silane (a=1, m=1, n=3);
Saturated alkyl dimethylethoxysilane class (a=1 such as n-pro-pyl dimethylethoxysilane, normal-butyl dimethylethoxysilane, positive decyl dimethylethoxysilane, n-hexadecyl dimethylethoxysilane, n-eicosane base dimethylethoxysilane, m=2, n=1);
Saturated alkyl diethyl Ethoxysilane class (a=1 such as n-pro-pyl diethyl Ethoxysilane, normal-butyl diethyl Ethoxysilane, positive decyl diethyl Ethoxysilane, n-hexadecyl diethyl Ethoxysilane, n-eicosane base diethyl Ethoxysilane, m=2, n=2);
Saturated alkyl dipropyl Ethoxysilane classes such as normal-butyl dipropyl Ethoxysilane, positive decyl dipropyl Ethoxysilane, n-hexadecyl dipropyl Ethoxysilane, n-eicosane base dipropyl Ethoxysilane (a=1, m=2, n=3);
Saturated alkyl dimethyl propylene TMOS class (a=1 such as n-pro-pyl dimethyl propylene TMOS, normal-butyl dimethyl propylene TMOS, positive decyl dimethyl propylene TMOS, n-hexadecyl dimethyl propylene TMOS, n-eicosane base dimethyl propylene TMOS, m=3, n=1);
Saturated alkyl diethyl propoxyl group silanes (a=1 such as n-pro-pyl diethyl propoxyl group silane, normal-butyl diethyl propoxyl group silane, positive decyl diethyl propoxyl group silane, n-hexadecyl diethyl propoxyl group silane, n-eicosane base diethyl propoxyl group silane, m=3, n=2);
Saturated alkyl dipropyl propoxyl group silanes such as normal-butyl dipropyl propoxyl group silane, positive decyl dipropyl propoxyl group silane, n-hexadecyl dipropyl propoxyl group silane, n-eicosane base dipropyl propoxyl group silane (a=1, m=3, n=3);
Saturated alkyl methyl dimethoxysilane class (a=2 such as n-pro-pyl methyl dimethoxysilane, n-butylmethyldimethoxyforane, positive decyl methyl dimethoxysilane, n-hexadecyl methyl dimethoxysilane, n-eicosane ylmethyl dimethoxy silane, m=1, n=1);
Saturated alkyl ethyl dimethoxy silanes (a=2 such as n-pro-pyl ethyl dimethoxy silane, normal-butyl ethyl dimethoxy silane, positive decyl ethyl dimethoxy silane, n-hexadecyl ethyl dimethoxy silane, n-eicosane base ethyl dimethoxy silane, m=1, n=2);
Saturated alkyl propyl group dimethoxy silanes such as normal-butyl propyl group dimethoxy silane, positive decyl propyl group dimethoxy silane, n-hexadecyl propyl group dimethoxy silane, n-eicosane base propyl group dimethoxy silane (a=2, m=1, n=3);
Saturated alkyl methyldiethoxysilane class (a=2 such as n-pro-pyl methyldiethoxysilane, normal-butyl methyldiethoxysilane, positive decyl methyldiethoxysilane, n-hexadecyl methyldiethoxysilane, n-eicosane ylmethyl diethoxy silane, m=2, n=1);
Saturated alkyl ethyl diethoxy silane class (a=2 such as n-pro-pyl ethyl diethoxy silane, normal-butyl ethyl diethoxy silane, positive decyl ethyl diethoxy silane, n-hexadecyl ethyl diethoxy silane, n-eicosane base ethyl diethoxy silane, m=2, n=2);
Saturated alkyl propyl group diethoxy silane classes such as normal-butyl propyl group diethoxy silane, positive decyl propyl group diethoxy silane, n-hexadecyl propyl group diethoxy silane, n-eicosane base propyl group diethoxy silane (a=2, m=2, n=3);
Saturated alkyl methyl dipropoxy silanes (a=2 such as n-pro-pyl methyl dipropoxy silane, normal-butyl methyl dipropoxy silane, positive decyl methyl dipropoxy silane, hexadecane ylmethyl dipropoxy silane, n-eicosane ylmethyl dipropoxy silane, m=3, n=1);
Saturated alkyl ethyl dipropoxy silanes (a=2 such as n-pro-pyl ethyl dipropoxy silane, normal-butyl ethyl dipropoxy silane, positive decyl ethyl dipropoxy silane, n-hexadecyl ethyl dipropoxy silane, n-eicosane base ethyl dipropoxy silane, m=3, n=2);
Saturated alkyl propyl group dipropoxy silanes such as normal-butyl propyl group dipropoxy silane, positive decyl propyl group dipropoxy silane, n-hexadecyl propyl group dipropoxy silane, n-eicosane base propyl group dipropoxy silane (a=2, m=3, n=3);
Saturated alkyl trimethoxy silane classes such as n-pro-pyl trimethoxy silane, normal-butyl trimethoxy silane, positive decyl trimethoxy silane, n-hexadecyl trimethoxy silane, n-eicosane base trimethoxy silane (a=3, m=1);
Saturated alkyl triethoxysilicane alkanes such as n-pro-pyl triethoxysilane, ne-butyltriethoxysilaneand, positive decyl triethoxysilane, n-hexadecyl triethoxysilane, n-eicosane ethyl triethoxy silicane alkane (a=3, m=2);
Saturated alkyl tripropoxy silanes such as n-pro-pyl tripropoxy silane, normal-butyl tripropoxy silane, positive decyl tripropoxy silane, n-hexadecyl tripropoxy silane, n-eicosane base tripropoxy silane (a=3, m=3) etc.These can use more than 2 kinds alone or in combination.
Wherein, preferred normal-butyl trimethoxy silane, positive decyl trimethoxy silane, n-hexadecyl trimethoxy silane, positive decyl dimethyl methyl TMOS, n-hexadecyl dimethyl methyl TMOS, ne-butyltriethoxysilaneand, positive decyl triethoxysilane, n-hexadecyl triethoxysilane, normal-butyl tripropoxy silane, positive decyl tripropoxy silane, n-hexadecyl tripropoxy silane etc.
Proportional as containing of the decane couplant in the film formation material layer of transfer film of the present invention, with respect to glass powder 100 weight portions, be preferably 0.001～10 weight portion, more preferably 0.001～5 weight portion.The ratio of decane couplant is during less than 0.001 weight portion, can not give full play to the flexual raising effect in the film formation material layer of raising effect, formation of the dispersion stabilization of glass powder.On the other hand, when this ratio surpassed 10 weight portions, when the glass paste composition that preservation obtains, viscosity rose in time sometimes, perhaps reacted between the decane couplant and became the reason that the light transmittance after burning till descends.
＜plasticizer 〉
For good pliability and the flammability of performance in the film formation material layer that forms, preferably in composition of the present invention, contain plasticizer.As this plasticizer, the preferred plasticizer that constitutes by compound with following formula (3) expression.
Figure C200480010919D00171
(in the formula, R 2And R 5The alkyl of representing identical or different carbon number 1～30 respectively, R 3And R 4The alkylene of representing identical or different methylene or carbon number 2～30 respectively, s are 0～5, and t is 1～10 number.)
According to the transfer film that possesses the film formation material layer that contains plasticizer, even with its warpage, small be full of cracks (crackle) can not take place on the surface of this film formation material layer, in addition yet, it is soft outstanding that this transfer film becomes, and also can easily it be batched to be the roller shape.
Particularly, because the plasticizer that is made of the compound with above-mentioned formula (3) expression is thermal decomposited removal easily, so the light transmittance of the dielectric layer that burns till this film formation material layer and obtain is reduced.
In above-mentioned formula (3), use R 2Or R 5The expression alkyl and use R 3Or R 4The alkylene of expression can be the straight chain shape, also can be the branch shape, in addition, can be saturated base, also can be unsaturated group.
Use R 2Or R 5The carbon number of alkyl of expression is 1～30, is preferably 2～20, more preferably 4～10.
The carbon number of this alkyl surpasses at 30 o'clock, and the dissolubility with respect to the plasticizer that constitutes solvent of the present invention can reduce sometimes, can not obtain good pliability.
As the object lesson of the compound of representing with above-mentioned formula (3), can enumerate dibutyl adipate, diisobutyl adipate, adipic acid two-2-Octyl Nitrite, azelaic acid two-2-Octyl Nitrite, dibutyl sebacate, adipic acid dibutyl binaryglycol ester etc.Preferred n is the compound of 2～6 expressions.
Proportional as containing of the plasticizer in the film formation material layer of transfer film of the present invention, with respect to glass powder 100 weight portions, be preferably 0.1～20 weight portion, more preferably 0.5～10 weight portion.The ratio of plasticizer can not fully improve the plasticity of film formation material layer during less than 0.1 weight portion sometimes.On the other hand, when this ratio surpasses 20 weight portions, use the composition that obtains sometimes and the adhesiveness (viscosity) of the film formation material layer that forms becomes excessive, possess the operability variation of the transfer film of such film formation material layer.
In composition of the present invention, except above-mentioned necessary composition, also tackifier, surface tension can be adjusted various additives such as agent, stabilizer, defoamer and contain as any composition.
＜radioactivity-sensitive composition 〉
The inorganic particulate composition that contains of the present invention also can be for containing the radioactivity-sensitive inorganic particulate composition of radioactivity-sensitive composition.As this radioactivity-sensitive composition, for example, can be with the combination of (a) polyfunctional monomer and radioactive ray polymerization initiator, (b) melmac and the combination etc. of light acid initator that forms acid by radiation exposure as preferred illustration, in the combination of above-mentioned (a), the combination of especially preferably multi-functional (methyl) acrylate and radioactive ray polymerization initiator
As the object lesson of multi-functional (methyl) acrylate that constitutes the radioactivity-sensitive composition, can enumerate two (methyl) esters of acrylic acid of alkylene glycols such as ethylene glycol, propylene glycol; Two (methyl) esters of acrylic acid of poly-alkylene glycols such as polyethylene glycol, polypropylene glycol; Two (methyl) esters of acrylic acid of two terminal hydroxyl fluidized polymers such as two terminal hydroxyl polybutadiene, two terminal hydroxyl polyisoprene, two terminal hydroxyl polycaprolactams;
Glycerol, 1,2, poly-(methyl) esters of acrylic acid of the polyalcohol that 3 valencys such as 4-butantriol, trihydroxy methyl chain alkane, tetra methylol chain alkane, pentaerythrite, dipentaerythritol are above; Accrete poly-(methyl) esters of acrylic acid of the poly-alkylene glycols of the polyalcohol that 3 valencys are above; Poly-(methyl) esters of acrylic acid of ring type such as 1,4-cyclohexanediol, 1,4-Benzenediol polyalcohol; Oligomerization (methyl) esters of acrylic acids such as polyester (methyl) acrylate, epoxy (methyl) acrylate, amino methyl ethyl ester (methyl) acrylate, alkyd resins (methyl) acrylate, silane resin (methyl) acrylate, spirane (methyl) acrylate etc.These can use more than 2 kinds alone or in combination.
In addition, object lesson as the radioactive ray polymerization initiator that constitutes the radioactivity-sensitive composition, can enumerate benzil, benzoin, Benzophenone, camphorquinone, 2-hydroxyl-2-methyl-1-phenyl the third-1-ketone, 1-hydroxycyclohexylphenylketone, 2,2-dimethoxy agent-2-phenyl acetophenone, 2-methyl-[4 '-(methyl mercapto) phenyl]-2-phenyl acetophenone, 2-benzyl-2-dimethylamino-1-(4-morphine base phenyl)-carboxyl compounds such as fourth-1 ketone; Azo-compound or triazo-compounds such as azodiisobutyronitrile, 4-phenylazide formaldehyde; Organosulfur compounds such as disulfide/thiol; Benzoyl peroxide, di-tert-butyl peroxide, tert-butyl hydroperoxide, cumene hydroperoxide, hydroperoxidation are to organic peroxides such as cumenes; 1,3-two (trichloromethyl)-5-(2 '-chlorphenyl)-1,3,5-triazine, 2-[2-(2-furyl) vinyl]-4,6-two (trichloromethyl)-1,3, haloform classes such as 5-triazine; 2,2 '-two (2-chlorphenyls) 4,5,4 ', 5 '-tetraphenyl 1, imidazoles dimers such as 2 '-di-imidazoles; Deng.These can use more than 2 kinds alone or in combination.
As an example that contains the inorganic particulate composition, form example if show preferred dielectric layer with composition, as inorganic particulate (glass powder), can enumerate by lead oxide, boron oxide, silica, calcium oxide (PbO-B 2O 3-SiO 2-CaO system) mixture 100 weight portions that constitute, as butyl methacrylate/ethylhexyl methacrylate/hydroxy propyl methacrylate/glycidyl methacrylate copolymer 5～30 weight portions of binding resin, as positive decyl trimethoxy agent silane 0.1～5 weight portion of dispersant, as adipic acid two-2-Octyl Nitrite 0.1～10 weight portion of plasticizer, as propylene glycol monomethyl ether 5～30 weight portions of solvent as the composition that must composition contains.
Composition of the present invention can be by using mixers such as roller mixer, blender, homogeneous blender to stir above-mentioned inorganic particulate, binding resin, specific compound and solvent and the modulation that becomes to assign to arbitrarily.
Tiao Zhi composition of the present invention is the paste composition with the flowability that is fit to coating as mentioned above, and its viscosity is generally 1,000～30, and 000mPas is preferably 3,000～10,000mPas.
Especially preferably use in the transfer film (transfer film of the present invention) that composition of the present invention can describe in detail below making.
In addition, composition of the present invention in the formation method by known film formation material layer in the past, be that silk screen print method etc. directly is coated on said composition on the surface of substrate, also can preferably use by dried coating film is formed in the method for film formation material layer.
＜transfer film 〉
Transfer film of the present invention is the preferred laminated film that uses in the formation operation of formation operation, the particularly dielectric layer of PDP inscape, possesses composition of the present invention is coated on the support film, constituted by the film formation material layer that dried coating film is formed.
That is, transfer film of the present invention forms the film formation material layer that contains inorganic particulate, binding resin and specific compound and constitutes on support film.
In addition, transfer film of the present invention also can be to form etchant resist described later on support film, is coated with composition of the present invention and the dry film (stacked film) that forms then thereon.
And then transfer film of the present invention also can be to use the radioactivity-sensitive transfer film that contains radioactivity-sensitive inorganic particulate composition and constitute.
(1) formation of transfer film:
Fig. 2 A is the fragmentary cross sectional view that expression is rolled into the transfer film of the present invention of roller shape, and Fig. 2 B is the sectional view [the part details drawing of Fig. 2 A] that the layer of this transfer film of expression constitutes.
Transfer film shown in Figure 2 is as an example of transfer film of the present invention, be the laminated film that is used to form the dielectric layer that constitutes PDP, usually by support film F1, constitute at the film formation material layer F2 that strippingly forms on the surface of this support film F1, the cover film F3 that on the surface of this film formation material layer F2, is easy to setting with peeling off.Sometimes also according to the character of film formation material layer F2 and do not use cover film F3.
The support film F1 that constitutes transfer film preferably has thermal endurance and solvent resistance and has flexual resin film.By making support film F1 have pliability, can use the composition (composition of the present invention) of coating pasty states such as roll coater, cutter coating machine, preserve established film formation material layer down with the state that is rolled into the roller shape when like this, can form the film formation material layer of thickness homogeneous and supply with.
As the resin that constitutes support film F1, for example can enumerate fluorine resins such as PETG, polyester, polyethylene, polypropylene, polystyrene, polyimides, polyvinyl alcohol, polyvinyl chloride, polyvinyl fluoride, nylon, cellulose etc.As the thickness of support film F1, for example be 20～100 μ m.
The film formation material layer F2 that constitutes transfer film is the layer that becomes glass sintering body (dielectric layer) by burning till, and glass powder (inorganic particulate), binding resin and specific compound are as containing by composition.
According to the kind of the containing ratio of glass powder, panel or size and difference, for example 5～200 μ m are preferably 10～100 μ m as the thickness of film formation material layer F2.This thickness is during less than 5 μ m, and the thickness of the final dielectric layer that forms is too small sometimes, can not guarantee the dielectric property of expecting.If this thickness is 5～200 μ m usually, then can guarantee the thickness of the dielectric layer of large-scale panel requirement fully.
The cover film F3 that constitutes transfer film is used for the film that diaphragm forms the surface (with the contact-making surface of glass substrate) of material layer F2.This cover film F3 also is preferably has flexual resin film.As the resin that forms cover film F3, can enumerate as the illustrative resin of resin that forms support film F1.As the thickness of cover film F3, for example be 20～100 μ m.
(1) manufacture method of transfer film:
Transfer film of the present invention can form film formation material layer (F2) by going up in support film (F1), cover film (F3) is set on this film formation material layer (F2), and (pressing sticking) makes.
As the formation method of film formation material layer, can enumerate the composition of the present invention that contains inorganic particulate, binding resin, dispersant, plasticizer and solvent is coated support film, made dried coating film to remove part or all method of solvent in early stage.
As the method for composition of the present invention being coated on the support film, from the outstanding viewpoint of filming of homogeneity of the thickness that can form thickness big (for example more than the 20 μ m), thickness effectively, as preferable methods can enumerate the coating process that utilizes roll coater, utilize the cutter coating machine of scraper etc. coating process, utilize curtain formula curtain coater coating process, utilize the coating process of cable coating machine etc.
Also have and preferably on the surface of the support film that is coated with composition of the present invention, implement demoulding processing.Like this, after transfer film forms material layer, can easily peel off support film from this film formation material layer.
Filming by part or all of drying removal solvent of the composition of the present invention that utilization forms on support film becomes the film formation material layer that constitutes transfer film.As the drying condition of filming that utilizes composition of the present invention, be about 0.1～30 minute under 40～150 ℃ for example.The remaining ratio of dried solvent (containing of the solvent in the film formation material layer is proportional) is generally below the 10 weight %, is preferably 0.1～5 weight % from the regulation of bringing into play the film formation material layer with respect to the base plate bonding and the shape retention of appropriateness.
Preferably implementing the demoulding on the surface of (usually by the heat pressure adhesive) cover film that is provided with on the film formation material layer that forms as mentioned above handles.Like this, before transfer film forms material layer, can easily peel off cover film from this film formation material layer.
(1) transfer printing of film formation material layer (using method of transfer film);
Film formation material layer on the support film is transferred to the surface of substrate together.Utilize transfer film of the present invention, owing to can on glass substrate, form the film formation material layer reliably by such shirtsleeve operation, improve (high efficiency) so can realize the operation in forming operation of inscape of the PDP of dielectric layer etc., can realize simultaneously the raising performance of the stable dielectric property of dielectric layer (for example) of the quality of the inscape that forms.
The manufacture method of＜PDP (1) (formation of dielectric layer) 〉
The manufacture method of PDP of the present invention (1) is included in that transfer printing constitutes the film formation material layer of transfer film of the present invention on the surface of substrate, forms the operation of dielectric layer by burning till the film formation material layer that is transferred on the surface of aforesaid substrate.
An example of the transfer printing process of the film formation material layer of the transfer film of utilization formation as shown in Figure 2 is shown as described below.
1. the transfer film that will be twisted in the state on the roller is cut off the size into the area of counterpart substrate.
2. from by film formation material layer (F2) the sur-face peeling cover film (F3) the transfer film of cutting off afterwards, overlapping transfer film on the surface of substrate is so that the surface butt joint of film formation material layer (F2).
3. mobile warm-up mill makes it bonding with hot pressing on the transfer film that is laminated on the substrate.
4. peel off removal support film (F1) from the film formation material layer (F2) that is fixed in by heat pressure adhesive on the substrate.
By as above-mentioned operation, the film formation material layer (F2) on the support film (F1) is needed on the substrate.Here, as the transfer printing condition, for example the surface temperature of warm-up mill is 60～120 ℃, to utilize the roll-in of warm-up mill be 1～5kg/cm 2, warm-up mill translational speed be 0.2～10.0m/ branch.Such operation (transfer printing process) can be undertaken by the laminating machine device.Also have, substrate can be preheated, and as preheat temperature, can be for example 40～100 ℃.
The film formation material layer (F2) that forms transfer printing on the surface of substrate is burnt till and is become inorganic sintered body (dielectric layer).Here, as process for calcining, can enumerate the substrate that film formation material layer (F2) transfer printing is formed and be disposed at method under the hot environment.Like this, decompose to remove the organic substance that in film formation material layer (F2), contains (binding resin for example.Residual solvent, dispersant, plasticizer, various additive), the inorganic particulate molten sintering.Wherein, as firing temperature, according to the melt temperature of substrate, the differences such as constitute in the film formation material layer, for example be 300～800 ℃, and then be preferably 400～600 ℃.
The manufacture method of＜PDP (2) (utilizing the formation of the inscape of photoresist method) 〉
PDP manufacture method of the present invention (2) comprises following operation: the film formation material layer that will constitute transfer film of the present invention is transferred on the substrate, on the film formation material layer of transfer printing, form etchant resist, this etchant resist of exposure-processed, form the sub-image of resist pattern, this etchant resist of development treatment, make the resist patterned surfacesization, this film formation material layer of etch processes, form and the corresponding patterned layer of resist pattern, handle this patterned layer by burning till, form from the next door, electrode, resistive element, dielectric layer, fluorophor, the inscape of selecting in colour filter and the black matrix.
In addition, also comprise following operation: on support film, form etchant resist and contain the film formation material layer that the inorganic particulate composition obtains by of the present invention, to be transferred on the substrate at the stacked film that forms on the support film, exposure-processed constitutes the etchant resist of this stacked film, form the sub-image of resist pattern, this etchant resist of development treatment, make the resist patterned surfacesization, this film formation material layer of etch processes, form and the corresponding patterned layer of resist pattern, handle this patterned layer by burning till, form from the next door, electrode, resistive element, dielectric layer, fluorophor, the inscape of selecting in colour filter and the black matrix.
Below, to form on the surface on the substrate overleaf as the inscape of PDP " next door " and method describe.In the method, transfer printing process, the formation operation of [2] etchant resist, the exposure process of [3] etchant resist, the developing procedure of [4] etchant resist, the etching work procedure of [5] film formation material layer, [6] by [1] film formation material layer form the next door by the formation operation of partition pattern on the surface of substrate.
Fig. 3 and Fig. 4 are the fragmentary cross sectional view that expression is used to form a series of operation in next door.In Fig. 3 and Fig. 4,11 is glass substrate, at the first-class electrode 12 that is used to make the plasma generation that is spaced of this glass substrate, forms dielectric layer 13 with coated electrode 12 on the surface of glass substrate 11.
Also have, in the present invention, as " " mode except the lip-deep mode of the above-mentioned glass substrate 11 of transfer printing, also comprises the lip-deep mode that is needed on above-mentioned dielectric layer 13 to transfer film formation material layer on substrate.
(1) transfer printing process of film formation material layer:
An example of the transfer printing process of film formation material layer is as described below.
The cover film (diagram omit) of peeling off transfer film afterwards, shown in Fig. 3 B, stacked transfer film 20 on the surface of dielectric layer 13 is so that the surface butt joint of film formation material layer 21,, peel off from film formation material layer 21 and to remove support film 22 should after the transfer film 20 by thermocompression bonded such as warm-up mill.Like this, shown in Fig. 3 C, transfer film forms material layer 21 on the surface of dielectric layer 13, becomes the state of adhesion.Here, as the transfer printing condition,, for example the surface temperature of warm-up mill is 80～140 ℃, to utilize the roll-in of warm-up mill be 1～5kg/cm 2, warm-up mill translational speed be 0.1～10.0m/ branch.In addition, glass substrate 11 can be preheated, and as preheat temperature, can be for example 40～100 ℃.
(1) the formation operation of etchant resist:
In this operation, shown in Fig. 3 D, on the surface of the film formation material layer that has been transferred, form etchant resist 31.As the resist that constitutes such etchant resist 31, can be any one of positive type resist and cloudy type resist.
Etchant resist 31 is moulded by silk screen print method, print roll coating method, method of spin coating, stream after the whole bag of tricks painting erosion resistant agent such as rubbing method, can form by making dried coating film.The baking temperature of here, filming is generally about 60～130 ℃.
In addition, also can form by the etchant resist that transfer printing on the surface of film formation material layer 21 has formed on support film.By such formation method, can reduce the formation process number of etchant resist, the thickness homogeneity of the resist that obtains simultaneously is outstanding, so can carry out the development treatment of this resist and the etch processes of film formation material layer equably, the height in the next door of formation and the shape homogeneous that becomes.
As the thickness of etchant resist 31, be generally 0.1～40 μ m, be preferably 0.5～20 μ m.
(1) exposure-processed of etchant resist:
In this operation, shown in Fig. 3 E, on the surface of the etchant resist 31 that forms on the film formation material layer 21, by exposure mask M, irradiation (exposure) ultraviolet isoradial optionally.Form the sub-image of resist pattern.In same figure, MA and MB are respectively transmittance section and the light shielding part among the exposure mask M.
Here, as ultraviolet lamp, the exposure device that uses when the ultraviolet lamp that uses with above-mentioned photoetching process manufacturing, semiconductor and the liquid crystal indicator etc. is not particularly limited.
Also have, when forming etchant resist, preferably under the state of not peeling off the support film that is covering on the etchant resist, carry out exposure-processed by transfer printing.
(1) development treatment of etchant resist
In this operation,, resist pattern (sub-image) is come to the surface by the etchant resist that development treatment has been exposed.
Here, as the development treatment condition, corresponding with kind of etchant resist 31 etc., can suit to select kind/composition/concentration, developing time, development temperature, developing method (for example infusion process, suspension system, shower method, splash method, paddle method), developing apparatus of developer solution etc.
By this developing procedure, shown in Fig. 4 A, form the resist pattern 35 (pattern corresponding) that constitutes by residual 35A of resist, the resist removal 35B of portion with exposure mask M.
This resist pattern 35 is the patterns as the etching mask effect in the next operation (etching work procedure), and the constituent material of residual 35A of resist (resist of photocuring) is compared little with respect to the dissolution velocity of etching solution by necessity with the constituent material of film formation material layer 21.
(1) etching work procedure of film formation material layer:
In this operation, etch processes film formation material layer forms the partition pattern layer corresponding with the resist pattern.
That is, shown in Fig. 4 B, corresponding with the resist removal 35B of portion of resist pattern 35 being partially dissolved in the etching solution and selected removal in the film formation material layer 21.Here, Fig. 4 B represents the state in the etch processes.
Then, if further continue etch processes, shown in Fig. 4 C, the part of the regulation in the film formation material layer 21 is fully removed, and dielectric layer 13 exposes.Like this, form the partition pattern layer 25 that constitutes by residual 25A of material layer, the material layer removal 25B of portion.
Here, as etch process conditions, corresponding with kind of film formation material layer 21 etc., can suit to select kind/composition/concentration, processing time, treatment temperature, processing method (for example infusion process, suspension system, shower method, splash method, paddle method), processing unit of etching solution etc.
Also have, residual the 35A of resist that preferably constitutes resist pattern 35 dissolves when etch processes gradually, removed fully in the stage that forms partition pattern layer 25 (when etch processes finishes).
Also have, even stay part or all of residual 35A after the etch processes, residual 35A of this resist also is removed in next firing process.
(1) firing process of partition pattern layer:
In this operation, burn till and handle partition pattern layer 25 formation next door.Like this, organic substance among residual 25A of material layer burns and loses and the formation next door, shown in Fig. 4 D, in the panel material 50 that formation next door 40 forms on the surface of dielectric layer 13, utilize the space (deriving from the space of the material layer removal 25B of portion) of next door 40 subregions to become the plasma effect space.
Here, as the temperature of burning till processing, it is necessary that the organic substance of residual 25A of material layer burns the temperature of losing, and is generally 400～600 ℃.In addition, firing time is generally 10～90 minutes.
The manufacture method of＜PDP (3) (utilizing the preferred implementation of photoresist method) 〉
The manufacture method of PDP among the present invention is not limited by as shown in Figure 3 and Figure 4 method.
As other method for optimizing that is used to form the PDP inscape (manufacture method of PDP 3.), can enumerate formation method here, by the operation of following (1)～(3).
(1) on support film, form after the etchant resist, on this etchant resist coating of the present inventionly contain the inorganic particulate composition, by dry stacked formation film formation material layer., when forming etchant resist and film formation material layer, roll coater etc. can be used here, like this, the outstanding stacked film of homogeneity of thickness can be on support film, formed.
(2) etchant resist that on support film, forms in transfer printing on the substrate and the stacked film of film formation material layer.Here, as the transfer printing condition, so long as with above-mentioned " transfer printing process of film formation material layer " and in identical the getting final product of condition.
(3) carry out and above-mentioned " exposure process of etchant resist ", " developing procedure of etchant resist ", " etching work procedure of film formation material layer " and " firing process of partition pattern layer " identical operations.At this moment, as previously mentioned, preferably making the developer solution of etchant resist is identical solution with the etching solution of film formation material layer, implements continuously " developing procedure of etchant resist " and " etching work procedure of film formation material layer ".
By as above-mentioned method since on substrate together transfer film form material layer and etchant resist, make efficient so can further improve by the simplification of operation.
The manufacture method of＜PDP (4) (using the formation of the inscape of radioactivity-sensitive transfer film) 〉
The manufacture method of PDP of the present invention (4) comprises following operation: the film formation material layer that will constitute radioactivity-sensitive transfer film of the present invention is transferred on the substrate, this film formation material layer of exposure-processed, form the sub-image of resist pattern, this film formation material layer of development treatment, form patterned layer, handle this patterned layer by burning till, form the inscape of from next door, electrode, resistive element, dielectric layer, fluorophor, colour filter and black matrix, selecting.
In the method, for example as an example with the formation method in next door, at " transfer printing process of film formation material layer " afterwards, under the condition that with above-mentioned " exposure process of etchant resist ", " developing procedure of etchant resist " is benchmark, form patterned layer, by " firing process of partition pattern ", on the surface of substrate, form the next door then.
In each specification of manufacture method (1)～(4) of above PDP, the method of formation as " next door " of PDP inscape is illustrated, but can is that benchmark forms electrode, resistive element, dielectric layer, fluorophor, colour filter and the black matrix etc. that constitute PDP also with this method.
＜embodiment 〉
Below embodiments of the invention are described, but the present invention is not limited by these embodiment.Also have, to following, " portion " expression " weight portion ".
Embodiment 1
(1) modulation of glass paste composition (containing the inorganic particulate composition):
As glass powder (inorganic particulate),, stir by lead oxide, boron oxide, silica, calcium oxide (PbO-B by using dispersion machine 2O 3-SiO 2-CaO system) mixture (560 ℃ of softening points) 100 weight portions that constitute, butyl methacrylate (BMA)/methacrylic acid 2-Octyl Nitrite (EHMA)/methacrylic acid 2-hydroxypropyl acrylate (HPMA)/glycidyl methacrylate (GMA) copolymer (weight ratio 30/60/5/5 as binding resin, weight average molecular weight 105,000) 17 weight portions, positive decyl trimethoxy agent silane 1.0 weight portions as dispersant, adipic acid two-2-Octyl Nitrite 2.5 weight portions as plasticizer, propylene glycol monomethyl ether 7.3 weight portions as solvent, ethyl-3-ethoxy-c acid esters, 11.5 weight portions, modulation viscosity is 1,600mPas (20rpm, eastern machine industry system, TV-30 type viscosimeter) composition of the present invention.
(2) manufacturing of transfer film and evaluation (pliability and operability):
Use the cutter coating machine, on the support film (width 400mm, length 30m, thickness 38 μ m) that the PETG (PET) that the demoulding in advance forms constitutes, be coated on the composition of the present invention of above-mentioned (1) modulation, by under 100 ℃, making established dried coating film 5 minutes to remove solvent, like this, on support film, form the film formation material layer of thickness 90 μ m.Then, the cover film (width 400mm, length 30m, thickness 38 μ m) that the PET that is handled by the demoulding in advance by attaching constitutes is made the transfer film of the present invention with formation as shown in Figure 2 on this film formation material layer.
The transfer film that obtains has flexibility, can easily batch the operation into the roller shape.In addition, even this transfer film of warpage also can not crack on the surface of film formation material layer (flexing be full of cracks), this film formation material layer has outstanding pliability.
In addition, peel off cover film from this transfer film, not to this transfer film duplexer of film formation material layer (support film with) and its overlapping so that surface of film formation material layer is docked with the surface of glass substrate, then, after glass substrate is peeled off this transfer film, this film formation material layer shows the adhesiveness of appropriateness with respect to glass substrate, and, can cohesion destruction not taken place on this film formation material layer and peel off transfer film, good as the operability (handling) of transfer film.
(3) transfer printing of film formation material layer:
After the transfer film that obtains by above-mentioned (2) is peeled off cover film, (stationary plane of bus electrode) goes up overlapping this transfer film duplexer of film formation material layer (support film with) so that dock on the surface of film formation material layer on the surface of the glass substrate that 21 inches panels are used, by the warm-up mill thermocompression bonded should transfer film.Here, as pressing stick spare, the surface temperature of warm-up mill is made as 90 ℃, roll-in is made as 2kg/cm 2, the translational speed of warm-up mill is made as the 0.8m/ branch.
After heat pressure adhesive finishes, peel off the removal support film in the lip-deep film formation material layer of glass substrate, finish the transfer printing of this film formation material layer from fixing (caking).
In this transfer printing process, when peeling off support film, the cohesion of film formation material layer can not take place destroy, this film formation material layer has fully big film-strength.And then the film formation material layer that has been transferred has good adhesiveness with respect to the surface of glass substrate.
(4) the burning till of film formation material layer (formation of dielectric layer):
The glass substrate of the film formation material layer that will be forms by above-mentioned (3) transfer printing is disposed in the firing furnace, ratio with 10 ℃ of per minutes makes the temperature in the stove above-mentioned after 570 ℃, handled 10 minutes by under 570 ℃, burning till, and on the surface of glass substrate, form the dielectric layer that constitutes by the glass sintering body.
The thickness (average film thickness and tolerance) of measuring this dielectric layer is the scope at 44 μ m ± 0.4 μ m, and the homogeneity of thickness is outstanding.
In addition, surface to the dielectric layer that obtains, use noncontact film thickness gauge (water chestnut light corporate system, NH-3) implements three-dimensional measurement, with JIS specification (B0601) is that benchmark is tried to achieve surface roughness (Ra, Ry, Rz), be Ra=0.06 μ m, Ry=0.43 μ m, Rz=0.21 μ m, surface smoothing is outstanding.
Embodiment 2～6
In embodiment 1, except use the copolymer shown in the table 1 respectively as binding resin, modulate the glass paste composition in the same manner with embodiment 1 (1), use each glass paste that obtains, be identically formed transfer film with embodiment 1 (2).The transfer film that obtains all has limpness, can easily batch the operation into the roller shape.In addition, even this transfer film of warpage also can not crack on the surface of film formation material layer (flexing be full of cracks), this film formation material layer has outstanding pliability.
Each transfer film that use obtains carries out transfer printing in the same manner with embodiment 1 (3), even when using any transfer film, when peeling off support film, the cohesion of film formation material layer can not take place yet destroy, and this film formation material layer has fully big film-strength.And then the film formation material layer that has been transferred has good adhesiveness with respect to the surface of glass substrate.
And then, be identically formed dielectric layer with embodiment 1 (4), to the surface of the dielectric layer that obtains, try to achieve surface roughness (Ra, Ry, Rz) in the same manner with embodiment 1.The value of Ra, Ry, Rz is illustrated in the table 1 jointly.
Table 1
Figure C200480010919D00291
Comparative example
The umber of binding resin is made as 17 parts, except replacing butyl methacrylate/methacrylic acid 2-Octyl Nitrite/methacrylic acid 2-hydroxypropyl acrylate/glycidyl methacrylate copolymer (weight ratio 30/60/5/5, weight average molecular weight 105,000) uses butyl methacrylate/methacrylic acid 2-Octyl Nitrite/methacrylic acid 2-hydroxypropyl acrylate copolymer (weight ratio 30/60/10, weight average molecular weight 150,000) in addition, similarly modulating viscosity with embodiment is 1, the composition of 200mPas (20rpm, eastern machine industry system, TV-30 type viscosimeter).The composition that use obtains, similarly make transfer film, estimate with embodiment, pliability and operability are good, try to achieve surface roughness (Ra, Ry, Rz) and similarly form dielectric layer with embodiment, be Ra=0.31 μ m, Ry=2.61 μ m, Rz=1.10 μ m, surface smoothing is relatively poor.
The present invention is had been described in detail with reference to specific execution mode, but in addition various changes or correction, this point is very clear for the practitioner. with can not breaking away from spirit of the present invention and scope
The present invention is based on the invention of the Japanese patent application (special be willing to 2003-119490) of on April 24th, 2003 application, here as with reference to and adopt its content.
Industrial application
Can play effect described as follows by composition of the present invention.
(1) in the firing process in low temperature/short time, can form well surface smoothness and go out The inscape of the PDP of look (for example next door, electrode, resistive element, dielectric layer, fluorophor, Colour filter and black matrix).
(2) can make the outstanding transfer film of pliability of film formation material layer.
(3) can make the transfer printing (with respect to the Thermoadhesive that adds of substrate) of film formation material layer Outstanding transfer film.
Can play effect described as follows by transfer film of the present invention.
(1) in the firing process in low temperature/short time, can effectively form surface smoothness and go out The inscape of the PDP of look (for example being dielectric layer).
(2) pliability of film formation material layer is outstanding, does not produce on the surface of this film formation material layer Flexing be full of cracks (crackle).
(3) soft outstanding, can easily batch the operation into the roller shape.
(4) the film formation material layer shows good cohesive, and operability (handling) is good.
(5) transfer printing of film formation material layer (with respect to the Thermoadhesive that adds of substrate) is outstanding.
Can play effect described as follows by manufacture method of the present invention.
(1) in the firing process in low temperature/short time, can effectively form surface smoothness and go out The inscape of the PDP of look (for example next door, electrode, resistive element, dielectric layer, fluorophor, Colour filter and black matrix).
(2) in the firing process in low temperature/short time, can effectively form the position of inscape Put the high PDP of precision.
(3) in the firing process in low temperature/short time, can effectively form the big electricity of thickness and be situated between The matter layer.
(4) in the firing process in low temperature/short time, can effectively form by large-scale panel and want The dielectric layer of asking.
(5) in the firing process in low temperature/short time, can effectively form possess thickness all The PDP of the dielectric layer that one property and surface smoothness are outstanding.

Claims (12)

1. an inorganic particle containing composition for plasma display panel is characterized in that,
Contain [A] inorganic particulate and [B] binding resin, this binding resin contains the polymer [B-1] that has with the repetitive of following formula (I) expression,
Figure C200480010919C00021
In the formula, X represents hydrogen atom or methyl, R 1Expression singly-bound, methylene or carbon number are that 2～5 alkylene, n represent 1～6 integer.
2. the inorganic particulate composition that contains according to claim 1 is characterized in that,
Further contain [C] radioactivity-sensitive composition.
3. the inorganic particulate composition that contains according to claim 1 is characterized in that,
Further contain plasticizer.
4. the inorganic particulate composition that contains according to claim 1 is characterized in that,
Further contain silane coupling agent.
5. the inorganic particulate composition that contains according to claim 1 is characterized in that,
[B-1] polymer carries out the copolymer that combined polymerization obtains for the monomer with following formula (i) expression with at least a kind that is selected from (methyl) alkyl acrylate, (methyl) acrylic acid hydroxy alkyl ester and (methyl) alkoxyalkyl acrylate,
Figure C200480010919C00022
In the formula, X, R 1Identical with the definition of n with above-mentioned formula (I).
6. the inorganic particulate composition that contains according to claim 1 is characterized in that,
As [A] inorganic particulate, contain softening point and be 350～700 ℃ glass powder.
7. a transfer film is characterized in that,
Have by claim 1 is described and contain the film formation material layer that the inorganic particulate composition obtains.
8. a transfer film is characterized in that,
Have etchant resist and contain the film formation material layer that the inorganic particulate composition obtains by claim 1 is described.
9. the manufacture method of a Plasmia indicating panel is characterized in that,
Has following operation: will contain the film formation material layer that the inorganic particulate composition obtains and be transferred on the substrate by claim 1 is described, and, on described substrate, form dielectric layer by burning till the film formation material layer of transfer printing.
10. the manufacture method of a Plasmia indicating panel is characterized in that,
Has following operation: will contain the film formation material layer that the inorganic particulate composition obtains and be transferred on the substrate by claim 1 is described, on the film formation material layer of transfer printing, form etchant resist, this etchant resist of exposure-processed, form the sub-image of resist pattern, this etchant resist of development treatment, make the resist patterned surfacesization, this film formation material layer of etch processes, form the patterned layer corresponding with the resist pattern, handle this patterned layer by burning till, form the inscape of from next door, electrode, resistive element, dielectric layer, fluorophor, colour filter and black matrix, selecting.
11. the manufacture method of a Plasmia indicating panel is characterized in that,
Have following operation: on support film, form etchant resist with by the described stacked film that contains the film formation material layer that the inorganic particulate composition obtains of claim 1, to be transferred on the substrate at the stacked film that forms on the support film, exposure-processed constitutes the etchant resist of this stacked film, form the sub-image of resist pattern, this etchant resist of development treatment, make the resist patterned surfacesization, this film formation material layer of etch processes, form the patterned layer corresponding with the resist pattern, handle this patterned layer by burning till, form from the next door, electrode, resistive element, dielectric layer, fluorophor, the inscape of selecting in colour filter and the black matrix.
12. the manufacture method of a Plasmia indicating panel is characterized in that,
Has following operation: will contain the film formation material layer that the inorganic particulate composition obtains and be transferred on the substrate by claim 2 is described, this film formation material layer of exposure-processed, form the sub-image of pattern, this film formation material layer of development treatment, form patterned layer, handle this patterned layer by burning till, form the inscape of from next door, electrode, resistive element, dielectric layer, fluorophor, colour filter and black matrix, selecting.
CNB2004800109193A 2003-04-24 2004-02-25 Inorganic particle containing composition for plasma display panel, transfer film and process for producing plasma display panel Expired - Fee Related CN100461328C (en)

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