WO2009099141A1 - Matériau pour la formation d'élément d'écran plat - Google Patents

Matériau pour la formation d'élément d'écran plat Download PDF

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Publication number
WO2009099141A1
WO2009099141A1 PCT/JP2009/051958 JP2009051958W WO2009099141A1 WO 2009099141 A1 WO2009099141 A1 WO 2009099141A1 JP 2009051958 W JP2009051958 W JP 2009051958W WO 2009099141 A1 WO2009099141 A1 WO 2009099141A1
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WIPO (PCT)
Prior art keywords
parts
group
forming material
solvent
silane compound
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PCT/JP2009/051958
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English (en)
Japanese (ja)
Inventor
Keisuke Yajima
Youhei Ooishi
Tarou Kanamori
Masayuki Motonari
Ryousuke Iinuma
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Jsr Corporation
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Priority to JP2009552512A priority Critical patent/JPWO2009099141A1/ja
Publication of WO2009099141A1 publication Critical patent/WO2009099141A1/fr

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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
    • H01J11/10—AC-PDPs with at least one main electrode being out of contact with the plasma
    • H01J11/12—AC-PDPs with at least one main electrode being out of contact with the plasma with main electrodes provided on both sides of the discharge space
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L83/00—Compositions of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon only; Compositions of derivatives of such polymers
    • C08L83/04—Polysiloxanes
    • 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
    • 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
    • H01J11/38—Dielectric or insulating layers
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J29/00—Details of cathode-ray tubes or of electron-beam tubes of the types covered by group H01J31/00
    • H01J29/86—Vessels; Containers; Vacuum locks
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J31/00—Cathode ray tubes; Electron beam tubes
    • H01J31/08—Cathode ray tubes; Electron beam tubes having a screen on or from which an image or pattern is formed, picked up, converted, or stored
    • H01J31/10—Image or pattern display tubes, i.e. having electrical input and optical output; Flying-spot tubes for scanning purposes
    • H01J31/12—Image or pattern display tubes, i.e. having electrical input and optical output; Flying-spot tubes for scanning purposes with luminescent screen
    • H01J31/123—Flat display tubes
    • H01J31/125—Flat display tubes provided with control means permitting the electron beam to reach selected parts of the screen, e.g. digital selection
    • H01J31/127—Flat display tubes provided with control means permitting the electron beam to reach selected parts of the screen, e.g. digital selection using large area or array sources, i.e. essentially a source for each pixel group
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G77/00—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
    • C08G77/04—Polysiloxanes
    • C08G77/14—Polysiloxanes containing silicon bound to oxygen-containing groups
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G77/00—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
    • C08G77/04—Polysiloxanes
    • C08G77/14—Polysiloxanes containing silicon bound to oxygen-containing groups
    • C08G77/18—Polysiloxanes containing silicon bound to oxygen-containing groups to alkoxy or aryloxy groups

Definitions

  • the present invention relates to a flat panel display member forming material used for forming a flat panel display member such as a dielectric layer or a partition wall.
  • FPD flat panel displays
  • PDP plasma display panels
  • FED field emission displays
  • the PDP forms a transparent electrode, encloses an inert gas such as argon or neon between two glass plates arranged close to each other, causes plasma discharge to light the gas, thereby causing the phosphor to emit light.
  • the FED is a display that displays information by causing a phosphor to emit light by emitting electrons from the cathode into a vacuum by applying an electric field and irradiating the electrons on the anode.
  • FIG. 1 is a schematic diagram showing a cross-sectional shape of an AC type PDP.
  • 101 and 102 are glass substrates arranged opposite to each other, 103 is a partition, and cells are partitioned by the glass substrate 101, glass substrate 102 and partition 103.
  • 104 is a transparent electrode fixed on the glass substrate 101
  • 105 is a bus electrode formed on the transparent electrode 104 for the purpose of reducing the resistance of the transparent electrode 104
  • 106 is an address electrode fixed on the glass substrate 102
  • 107 is Fluorescent material held in the cell
  • 108 and 109 are dielectric layers formed on the surface of the glass substrate 101 so as to cover the bus electrode 105
  • 110 is a protective film made of, for example, magnesium oxide
  • 111 is a partition.
  • FIG. 2 is a schematic diagram showing the cross-sectional shape of the FED.
  • 201 and 202 are glass substrates
  • 203 is an insulating layer
  • 204 is a transparent electrode
  • 205 is an emitter
  • 206 is a cathode electrode
  • 207 is a phosphor
  • 208 is a gate
  • 209 is a spacer.
  • a method for producing such members as dielectrics, partition walls, electrodes, phosphors, color filters, and black stripes (matrix) used in such FPDs, for example, after forming an inorganic powder-containing resin layer on a substrate
  • a method of firing this see Patent Document 1 is known.
  • materials that can form members by processing at relatively low temperatures have been studied in response to the recent demand for cost reduction for FPDs (see Patent Documents 2 and 3).
  • an object of the present invention is to provide a material capable of obtaining an FPD member that is free from cracks and has both high heat resistance and transparency. Furthermore, an object of the present invention is to provide a material capable of obtaining a highly smooth member with a small number of coatings.
  • the flat panel display member forming material of the present invention includes silica particles (A), Following formula (1) R 1 n Si (OR 2 ) 4-n (1) (Wherein, R 1 represents a monovalent organic group having 1 to 8 carbon atoms, optionally .R 2 be different be the same as each other if there are two or more are each independently, Represents an alkyl group having 1 to 5 carbon atoms or an acyl group having 1 to 6 carbon atoms, n is an integer of 0 to 3)
  • inorganic particles other than the silica particles (A) may be contained.
  • the total amount of the silica particles (A) and the inorganic particles in terms of solid content and the amount of complete hydrolysis condensate of the silane compound (B) is 100 parts by mass.
  • the thickener (C) is preferably 0.05 to 30 parts by mass.
  • the flat panel display member forming material of the present invention contains, as the silica particles (A), particles having a particle diameter in the range of 0.03 to 0.3 ⁇ m measured by a laser diffraction method at 50% or more on a volume basis. It is preferable to use silica particles.
  • the said silica particle (A) and the said inorganic particle are 65 to less than 100 mass parts in conversion of solid content, and the said silane compound (B) is a complete hydrolysis condensation. More than 0 parts by mass and 35 parts by mass or less (however, the total amount of silica particles (A) and inorganic particles in terms of solid matter and the total amount of silane compound (B) in terms of complete hydrolysis condensate is 100 parts by mass) It is preferable to contain.
  • the flat panel display member forming material of the present invention is suitable as a material for forming a dielectric layer in a flat panel display.
  • a flat panel display member-forming material that is not cracked during the formation of a thick film, is excellent in transparency and heat resistance, and has a high smoothness and can be obtained with a small number of coatings.
  • the flat panel display member forming material (hereinafter also referred to as “FPD member forming material”) according to the present invention contains silica particles (A), a silane compound (B), and a thickener (C). It is.
  • Silica particles (A) used in the present invention is a powder, an aqueous sol or colloid dispersed in water, or a solvent sol or colloid dispersed in a polar solvent such as isopropyl alcohol or a nonpolar solvent such as toluene. Can be used in form.
  • silica particles are used in the form of a solvent-based sol or colloid, depending on the dispersibility of the silica particles, they may be further diluted with water or a solvent, and surface treatment is performed to improve the dispersibility. It may be used.
  • the solid content concentration is usually more than 0% by mass and 50% by mass or less, preferably 0.01 to 40% by mass or less.
  • colloidal silica dispersed in an organic solvent because the transparency and heat resistance of the resulting member are further improved.
  • # 150, # 200, # 300 manufactured by Nippon Aerosil Co., Ltd. can be used as the silica particles whose surface is not treated, and R972, R974, R976 manufactured by Nippon Aerosil Co., Ltd. are used as the silica whose surface has been hydrophobized.
  • RX200, RX300, RY200S, RY300, R106, SS50A manufactured by Tosoh Corporation, silo hovic 100 of Fuji Silysia, and the like can be used.
  • solvent-dispersed colloidal silica examples include alcohol-based solvent-dispersed colloidal silica such as isopropyl alcohol, ketone-based solvent-dispersed colloidal silica such as methylisobutyl, non-polar solvent-dispersed colloidal silica such as toluene, etc. are used. be able to.
  • the colloidal silica particles may be added at the time of hydrolysis condensation or may be added at the time of preparing the FPD member forming material.
  • particle diameter of silica particles As silica particles used in the present invention, particles having a particle diameter in the range of 0.03 to 0.3 ⁇ m are usually contained in an amount of 50% or more, preferably 60% or more, more preferably 70% or more on a volume basis. Those are preferred.
  • the particle size distribution of the silica particles is measured by a laser diffraction method using a particle size distribution measuring device (eg, Nanotrack particle size distribution measuring device UPA-150 manufactured by Nikkiso Co., Ltd.) in a state where the silica particles are dispersed in an organic solvent. can do.
  • a particle size distribution measuring device eg, Nanotrack particle size distribution measuring device UPA-150 manufactured by Nikkiso Co., Ltd.
  • the film When the content of particles having a particle size in the range of 0.03 to 0.3 ⁇ m is 50% or less on a volume basis due to the inclusion of particles having a particle size of 0.03 ⁇ m or less, the film may have a high Cracks may occur during use underneath. On the other hand, when the content of particles having a particle diameter in the range of 0.03 to 0.3 ⁇ m is 50% or less on a volume basis by containing particles having a particle diameter of 0.3 ⁇ m or more, the resulting member Transparency may be reduced. If the content of particles having a particle size in the range of 0.03 to 0.3 ⁇ m is 50% or more on a volume basis, particles having a plurality of particle size distributions may be mixed.
  • inorganic particles other than silica particles can be used.
  • other inorganic particles include ZrO 2 , Al 2 O 3 , AlGaAs, Al (OH) 3 , Sb 2 O 5 , Si 3 N 4 , Sn—In 2 O 3 , and Sb—In 2.
  • the inorganic particles can be used alone or in combination of two or more or as a composite of these inorganic compounds.
  • the content of the inorganic particles is preferably less than 40 parts by mass, more preferably less than 30 parts by mass when the total of the silica particles (A) and the inorganic particles is 100 parts by mass. .
  • content of the said inorganic particle exists in the said range, possibility that it will have a bad influence on an optical characteristic can be made low.
  • the FPD member forming material of the present invention can be particularly preferably used as a material for forming a dielectric layer in an FPD because the cured body has high transparency and can form a thick film.
  • the flat panel display member forming material of the present invention has the following formula (1): R 1 n Si (OR 2 ) 4-n (1) (Wherein, R 1 represents a monovalent organic group having 1 to 8 carbon atoms, optionally .R 2 be different be the same as each other if there are two or more are each independently, Represents an alkyl group having 1 to 5 carbon atoms or an acyl group having 1 to 6 carbon atoms, n is an integer of 0 to 3) And at least one silane compound (B) selected from the group consisting of hydrolysates and condensates of organosilanes (hereinafter also referred to as “specific organosilanes”).
  • R 1 is a monovalent organic group having 1 to 8 carbon atoms. Specific examples thereof include methyl group, ethyl group, n-propyl group, i-propyl group.
  • Alkyl groups such as a group, n-butyl group, i-butyl group, sec-butyl group, t-butyl group, n-hexyl group, n-heptyl group, n-octyl group, 2-ethylhexyl group; Acyl groups such as acetyl group, propionyl group, butyryl group, valeryl group, benzoyl group, trioyl group, caproyl group; Examples thereof include a vinyl group, an allyl group, a cyclohexyl group, a phenyl group, an epoxy group, a glycidyl group, a (meth) acryloxy group, a ureido group, an amide group, a fluoroacetamide group, and an isocyanate group.
  • examples of R 1 include substituted derivatives of the above organic groups.
  • substituent of the substituted derivative of R 1 include a halogen atom, a substituted or unsubstituted amino group, a hydroxyl group, a mercapto group, an isocyanate group, a glycidoxy group, a 3,4-epoxycyclohexyl group, and a (meth) acryloxy group.
  • the number of carbon atoms of R 1 composed of these substituted derivatives is preferably 8 or less including the carbon atoms in the substituent.
  • R 2 is an alkyl group having 1 to 5 carbon atoms or an acyl group having 1 to 6 carbon atoms.
  • the alkyl group having 1 to 5 carbon atoms include methyl group, ethyl group, n-propyl group, i-propyl group, n-butyl group, sec-butyl group, t-butyl group, and n-pentyl group.
  • the acyl group having 1 to 6 carbon atoms include acetyl group, propionyl group, butyryl group, valeryl group, caproyl group and the like.
  • the hydrolyzate and / or condensate of the above specific organosilane is used as the silane compound (B).
  • the silane compound (B) may be a single hydrolyzate and / or condensate of the above specific organosilane, or two or more hydrolyzates and / or condensates of the above specific organosilane. There may be.
  • This silane compound (B) is a compound in which a silanol group in a hydrolyzate produced by hydrolysis of the specific organosilane is condensed to form a Si—O—Si bond.
  • the hydrolyzate may be one in which at least one of 1 to 4 OR 2 groups contained in the specific organosilane is hydrolyzed.
  • one OR 2 group In which two or more OR 2 groups are hydrolyzed, or a mixture thereof.
  • all silanol groups do not need to be condensed, and include those in which some silanol groups are condensed, those in which most or all silanol groups are condensed, and mixtures thereof.
  • the catalyst used for the hydrolysis / condensation of the specific organosilane includes basic compounds, acidic compounds, organometallic compounds and / or partial hydrolysates thereof (hereinafter referred to as organometallic compounds and / or partial hydrolysates thereof).
  • the decomposition products are collectively referred to as “organometallic compounds”).
  • organometallic compounds as such a catalyst, for example, those described in paragraphs [0065] to [0078] of JP-A No. 2001-192615 can be used. Of these, basic compounds are preferred.
  • Basic compounds examples include ammonia (including ammonia aqueous solution), organic amine compounds, alkali metals such as sodium hydroxide and potassium hydroxide, hydroxides of alkaline earth metals, alkalis such as sodium methoxide and sodium ethoxide. Examples thereof include metal alkoxides. Of these, ammonia and organic amine compounds are preferred.
  • the organic amine include alkylamine, alkoxyamine, alkanolamine, and arylamine.
  • alkylamine include methylamine, ethylamine, propylamine, butylamine, hexylamine, octylamine, N, N-dimethylamine, N, N-diethylamine, N, N-dipropylamine, N, N-di Examples thereof include alkylamines having an alkyl group having 1 to 4 carbon atoms such as butylamine, trimethylamine, triethylamine, tripropylamine, and tributylamine.
  • Such basic compounds may be used singly or in combination of two or more. Of these, triethylamine, tetramethylammonium hydroxide, and pyridine are particularly preferable.
  • Acid compound Organic acids and inorganic acids can be used as the acidic compound. Such acidic compounds can be used singly or in combination of two or more. Of these acidic compounds, maleic acid, maleic anhydride, methanesulfonic acid, and acetic acid are particularly preferred.
  • organometallic compounds include the following formula (2): M (OR 10 ) r (R 11 COCHCOR 12 ) s (2) (Wherein M represents at least one metal atom selected from the group consisting of zirconium, titanium, aluminum and sodium, and R 10 and R 11 each independently represents a methyl group, an ethyl group, or an n-propyl group) A monovalent carbon having 1 to 6 carbon atoms such as a group, i-propyl group, n-butyl group, sec-butyl group, t-butyl group, n-pentyl group, n-hexyl group, cyclohexyl group, phenyl group, etc.
  • R 12 represents a monovalent hydrocarbon group having 1 to 6 carbon atoms, or methoxy group, ethoxy group, n-propoxy group, i-propoxy group, n-butoxy group, sec-butoxy Represents an alkoxyl group having 1 to 16 carbon atoms such as a group, t-butoxy group, lauryloxy group, stearyloxy group, and r and s are each independently an integer of 0 to 4, and (r + s) (Which satisfies the relationship of M valence)) (hereinafter referred to as “organometallic compound (2)”) 1 to 2 alkyl groups having 1 to 10 carbon atoms in one tin atom Examples thereof include a bonded tetravalent tin organometallic compound (hereinafter referred to as “organotin compound”) or a partial hydrolyzate thereof.
  • organotin compound (2) 1 to 2 alkyl groups having 1 to 10 carbon atoms in one tin atom Examples
  • the organotin compound a tetravalent tin organometallic compound in which one or two alkyl groups having 1 to 10 carbon atoms are bonded to one tin atom can be used.
  • Tin compounds organic tin oxides such as (C 4 H 9 ) 2 SnO, (C 8 H 17 ) 2 SnO, and ester compounds such as these organic tin oxides and silicates, dimethyl maleate, diethyl maleate, dioctyl phthalate And the reaction product.
  • the amount of the hydrolysis condensation catalyst used is usually 0.001 to 20 parts by weight, preferably 0.01 to 10 parts by weight, based on 100 parts by weight of the total of organosilane monomers (in terms of complete hydrolysis condensate), The amount is preferably 0.1 to 5 parts by mass.
  • the amount of water added at this time is usually 10 to 500 parts by mass, preferably 20 to 200 parts by mass, more preferably 30 to 30 parts by mass with respect to 100 parts by mass of the total of organosilane monomers (in terms of complete hydrolysis condensate). 100 parts by mass. It is preferable that the amount of water added be in the above range because the hydrolysis / condensation reaction proceeds sufficiently and the amount of water removed after the reaction is small.
  • the hydrolysis / condensation is preferably performed in an organic solvent.
  • organic solvent alcohols, aromatic hydrocarbons, ethers, ketones, esters and the like can be used.
  • the alcohols include methanol, ethanol, n-propyl alcohol, i-propyl alcohol, i-butyl alcohol, n-butyl alcohol, sec-butyl alcohol, t-butyl alcohol, n-hexyl alcohol, n- Examples include octyl alcohol, ethylene glycol, diethylene glycol, triethylene glycol, ethylene glycol monobutyl ether, ethylene glycol monoethyl ether acetate, diethylene glycol monoethyl ether, propylene glycol monomethyl ether, propylene monomethyl ether acetate, and diacetone alcohol.
  • aromatic hydrocarbons include benzene, toluene, xylene and the like.
  • ethers include tetrahydrofuran and dioxane.
  • ketones include acetone, methyl ethyl ketone, methyl isobutyl ketone, diisobutyl ketone and the like.
  • esters include ethyl acetate, propyl acetate, butyl acetate, propylene carbonate, methyl lactate, ethyl lactate, normal propyl lactate, isopropyl lactate, methyl 3-ethoxypropionate, ethyl 3-ethoxypropionate, and the like. It is done.
  • organic solvents can be used alone or in combination of two or more.
  • organic solvents other than alcohols such as methyl ethyl ketone, methyl isobutyl ketone, toluene, and xylene are preferably used from the viewpoint of promoting the reaction.
  • the above organic solvent can be appropriately used for the purpose of controlling hydrolysis and condensation reactions.
  • the amount used can be appropriately set according to desired conditions.
  • the temperature of the hydrolysis / condensation reaction is preferably 10 to 100 ° C., more preferably 15 to 80 ° C., and particularly preferably 20 to 70 ° C.
  • the reaction time is preferably 0.3 to 48 hours, more preferably 0.5 to 24 hours, and particularly preferably 1 to 12 hours.
  • inorganic particles such as silica may be included.
  • colloidal silica when hydrolyzing and condensing a specific organosilane, it is necessary if the acid used during the production of the colloidal silica remains, the acid also acts as a hydrolysis catalyst. The amount of catalyst added may be reduced according to the above.
  • the silane compound obtained by the hydrolysis / condensation reaction of the specific organosilane is preferably washed with water as a decatalyzing step after the hydrolysis / condensation reaction from the viewpoint of storage stability.
  • a basic compound is used as a catalyst, it is more preferable to carry out water washing after neutralization with an acidic compound after the reaction.
  • the above acidic compound can be used.
  • the amount of the acidic compound used is usually 0.5 to 2 bases, preferably 0.8 to 1.5 bases, more preferably 0.9 to 1. bases relative to 1 base of the basic compound used in the hydrolysis / condensation reaction. Three bases. It is preferable to use a water-soluble acidic compound because the acidic compound is easily extracted into the aqueous layer at the time of washing with water.
  • the acidic compound is usually added in an amount of 0.5 to 100 parts by weight, preferably 1 to 50 parts by weight, more preferably 2 to 10 parts by weight with respect to 100 parts by weight of water. .
  • the water used for the water washing after the neutralization treatment is usually 10 to 500 parts by weight, preferably 20 to 300 parts by weight, more preferably 30 to 200 parts by weight when the total amount of the specific organosilane used is 100 parts by weight. It is.
  • Washing with water is performed by adding water and stirring sufficiently, and then allowing to stand, and after confirming phase separation between the aqueous phase and the organic solvent phase, removing the lower layer moisture.
  • the number of washings is preferably 1 or more times, more preferably 2 or more times. Thereafter, the solvent is distilled off to obtain a hydrolyzate of organosiloxane.
  • Weight average molecular weight of silane compound (B) The weight average molecular weight (Mw) of the silane compound (B) obtained by the above hydrolysis / condensation is 800 to 50,000, preferably 1,000 to 40, in terms of polystyrene measured by gel permeation chromatography. , 000.
  • Mw weight average molecular weight
  • polysiloxane obtained from halogenated silane can also be used as the silane compound (B).
  • This polysiloxane does not need to have all the halogens eliminated and condensed, but some of the halogens eliminated and condensed, most (including all) halogens condensed and condensed, halogens
  • a group in which a group is modified with an alkoxy group by alcohol, a group in which a halogen group is partially hydrolyzed with water to a silanol group, and a mixture thereof are also included.
  • an organosilane in which a is usually 0 or more and 2 or less, preferably 0 or more and 1.8 or less.
  • a is in the above range, a coating film having excellent heat resistance can be obtained.
  • the value of a can be set by adjusting suitably the kind of said organosilane, and its mixture ratio.
  • R 3 is a monovalent organic group having 1 to 8 carbon atoms, and specific examples thereof include methyl group, ethyl group, n-propyl group, i-propyl group, n Alkyl groups such as -butyl, i-butyl, sec-butyl, t-butyl, n-hexyl, n-heptyl, n-octyl and 2-ethylhexyl; Acyl groups such as acetyl group, propionyl group, butyryl group, valeryl group, benzoyl group, trioyl group, caproyl group; Examples thereof include a vinyl group, an allyl group, a cyclohexyl group, a phenyl group, an epoxy group, a glycidyl group, a (meth) acryloxy group, a ureido group, an amide group, a fluoroacetamide group, and
  • examples of R 3 include substituted derivatives of the above organic groups.
  • examples of the substituent of the substituted derivative of R 3 include a halogen atom, a substituted or unsubstituted amino group, a hydroxyl group, a mercapto group, an isocyanate group, a glycidoxy group, a 3,4-epoxycyclohexyl group, a (meth) acryloxy group, A ureido group, an ammonium base, etc. are mentioned.
  • the number of carbon atoms of R 3 composed of these substituted derivatives is preferably 8 or less including the carbon atoms in the substituent.
  • the above average composition formula (3) when a plurality of R 3 are present, they may be the same or different.
  • R 4 is an alkyl group having 1 to 5 carbon atoms or an acyl group having 1 to 6 carbon atoms.
  • the alkyl group having 1 to 5 carbon atoms include methyl group, ethyl group, n-propyl group, i-propyl group, n-butyl group, sec-butyl group, t-butyl group, and n-pentyl group.
  • the acyl group having 1 to 6 carbon atoms include formyl group, acetyl group, propionyl group, butyryl group, valeryl group, trioyl group, caproyl group and the like. In the above formula (2), when a plurality of R 4 are present, they may be the same or different.
  • polysiloxane as a silane compound (B) in this invention.
  • examples of such polysiloxane include MKC silicate manufactured by Mitsubishi Chemical Corporation, ethyl silicate manufactured by Colcoat, silicone resin manufactured by Toray Dow Corning Silicone Co., Ltd., manufactured by Momentive Performance Materials Japan GK. Terminal hydroxypolysiloxane resin (for example, trade name YR3370), silicone resin manufactured by Shin-Etsu Chemical Co., Ltd., and the like.
  • Examples of the silane compound (B) in the present invention include a hydrolysis / condensation product of dimethyldimethoxysilane, a hydrolysis / condensation product of methyltrimethoxysilane, and a co-hydrolysis / condensation product of dimethyldimethoxysilane and methyltrimethoxysilane. It can be preferably used.
  • the content of the silica particles (A), the other inorganic particles, and the silane compound (B) is the solid content equivalent amount of the silica particles (A) and the other inorganic particles.
  • the total amount of the solids content of the particles and the total hydrolysis condensate of the silane compound (B) is 100 parts by mass
  • the total of the solids content of the silica particles (A) and other inorganic particles Is preferably 65 parts by mass or more and less than 100 parts by mass, more preferably 70 parts by mass or more and 98 parts by mass or less.
  • the flat panel display member forming material of the present invention contains a thickener (C).
  • a thickener (C) By containing such a thickener (C), the film formability can be improved when forming a film with a slit coater or the like.
  • the thickener (C) is 0.05 to 30 parts by mass with respect to a total of 100 parts by mass of the silica particles (A), the inorganic particles, and the silane compound (B). Preferably, it is contained in a proportion in the range of 1 to 20 parts by mass. When this ratio is 0.05 parts by mass or less, cracks may easily occur after film formation. On the other hand, when this ratio exceeds 30 parts by mass, the thickener tends to remain in the film after the thermal decomposition treatment, and the film is colored after firing, which is not preferable for use as a flat panel display member.
  • the ratio of the thickener (C) is 100 W C / (W A + W B ) [W A is the mass of the inorganic particles (A) in the FPD member forming material, W B is the mass of the silane compound (B) in the FPD member forming material, W C is the mass of the thickener (C) in the FPD member forming material. ] It is a value calculated by.
  • a thickener (C) As such a thickener (C), a polymer, a surfactant, an organic filler, an inorganic filler, and the like can be used, and it is particularly preferable to use a polymer.
  • a substance that is completely oxidized and removed by a firing temperature (400 to 600 ° C.) at the time of forming an FPD member is preferable. Is preferably used.
  • Polymers suitable as the thickener (C) include, for example, acrylic polymers, cellulose derivatives, polyvinyl alcohol, polyvinyl butyral, polyalkylene glycols such as polyethylene glycol and polypropylene glycol, copolymers thereof, and urethane heavy polymers. Examples thereof include a polymer, a melamine polymer, a homopolymer of lactic acid, a copolymer of lactic acid and a copolymerizable monomer, and these can be used alone or in combination of two or more.
  • the polymer used as the thickener (C) is preferably an acrylic polymer, a cellulose derivative, or a random copolymer of ethylene glycol-propylene glycol.
  • acrylic polymer a homopolymer of a (meth) acrylate compound represented by the following formula (4), two or more copolymers of a (meth) acrylate compound represented by the following formula (4), and A copolymer of a (meth) acrylate compound represented by the following formula (4) and another copolymerizable monomer is included.
  • R 5 represents a hydrogen atom or a methyl group
  • R 6 represents a monovalent organic group
  • the (meth) acrylate compound represented by the above formula (4) include methyl (meth) acrylate, ethyl (meth) acrylate, propyl (meth) acrylate, isopropyl (meth) acrylate, butyl (meth) acrylate, Isobutyl (meth) acrylate, t-butyl (meth) acrylate, pentyl (meth) acrylate, amyl (meth) acrylate, isoamyl (meth) acrylate, hexyl (meth) acrylate, heptyl (meth) acrylate, octyl (meth) acrylate, Isooctyl (meth) acrylate, 2-ethylhexyl (meth) acrylate, nonyl (meth) acrylate, decyl (meth) acrylate, isodecyl (meth) acrylate, undecy
  • the group represented by R 6 is preferably an alkyl group, an alkoxyalkyl group or a hydroxyalkyl group, and as a particularly preferred (meth) acrylate compound, methyl (meth) acrylate, Mention may be made of n-butyl (meth) acrylate, i-butyl (meth) acrylate 2-ethylhexyl (meth) acrylate, lauryl (meth) acrylate, isodecyl (meth) acrylate and 2-ethoxyethyl (meth) acrylate.
  • the other copolymerizable monomer used for copolymerization with the (meth) acrylate compound is not particularly limited as long as it is a compound copolymerizable with the (meth) acrylate compound.
  • (meth) acrylic acid And unsaturated carboxylic acids such as vinyl benzoic acid, maleic acid, and vinyl phthalic acid
  • vinyl group-containing radical polymerizable compounds such as vinyl benzyl methyl ether, vinyl glycidyl ether, styrene, ⁇ -methyl styrene, butadiene, and isoprene. .
  • Cellulose derivatives include methyl cellulose, ethyl cellulose, hydroxymethyl cellulose, 2-hydroxyethyl cellulose, 2-hydroxypropyl cellulose, 2-hydroxyethyl methylcellulose, 2-hydroxyethyl ethylcellulose, 2-hydroxypropyl methylcellulose, 2-hydroxypropyl ethylcellulose. And carboxymethylcellulose.
  • polyethylene glycol, polypropylene glycol, ethylene glycol / propylene glycol copolymer, and the like can be used as the polyalkylene glycol and its copolymer.
  • the molecular weight of the polyalkylene glycol and the copolymer thereof is preferably 200,000 or more, particularly preferably 500,000 or more.
  • the organic solvent (D) can be added for the purpose of adjusting the total solid content concentration and viscosity of the FPD member forming material, or adjusting the thickness of the resulting member. Moreover, the dispersion stability and storage stability of the obtained FPD member forming material can be further improved by adding an organic solvent (D).
  • an organic solvent used, the amount used can be appropriately set according to desired conditions.
  • the total solid content concentration of the obtained FPD member forming material is preferably 5 to 99% by mass, The amount is more preferably 7 to 95% by mass, particularly preferably 10 to 90% by mass.
  • the “solid content concentration” indicates the concentration of components other than the organic solvent in the entire FPD member forming material.
  • Examples of the organic solvent (D) include alcohols, hydrocarbons, ethers, ketones / aldehydes, polyhydric alcohols and their derivatives, which are exemplified as the organic solvent used in the production of the silane compound (B). Can do. Moreover, these organic solvents may be used individually by 1 type, or may mix and use 2 or more types.
  • the organic solvent (D) preferably has a boiling point at 1 atm of 100 ° C. or higher and 300 ° C. or lower, particularly preferably 150 ° C. or higher and 250 ° C. or lower. When the boiling point of the organic solvent is 100 ° C. or less, the material applied during the coating operation is likely to be rapidly dried, and the dried product adheres to the surface to be coated or uneven coating occurs. Sometimes. On the other hand, when the boiling point of the organic solvent exceeds 300 ° C., the organic solvent (D) tends to remain in the film after the baking treatment, which may cause a decrease in film strength and a rough surface of the coating film.
  • alcohols include 1-pentanol, 2-pentanol, 2-methyl-2-butanol, 3-methyl-1-butanol, 2-ethylbutanol, n-hexanol (n-hexyl alcohol), 2-ethylhexanol, 2-octanol, terpineol, i-butyl alcohol, n-butyl alcohol, n-octyl alcohol, 2-heptyl alcohol, ethylene glycol, ethylene glycol diacetate, ethylene glycol diethyl ether, ethylene glycol dimethyl ether, diethylene glycol, Triethylene glycol, ethylene glycol monobutyl ether (2-butoxyethanol), ethylene glycol monobutyl ether acetate, ethylene glycol monohexyl ether, Lenglycol monoethyl ether acetate, ethylene glycol monomethyl ether acetate, diethylene glycol monoethyl ether, diethylene glycol dieth
  • aromatic hydrocarbons include toluene and xylene.
  • ethers include diethyl acetal, dibutyl ether, dioxane and the like.
  • ketones include acetylacetone, ethyl-n-butylketone, diacetone alcohol, methylisobutylketone, methyl-n-butylketone, methyl-n-propylketone, diethylketone, diisobutylketone, diisopropylketone and the like.
  • esters include ethyl acetoacetate, methyl acetoacetate, ethyl benzoate, methyl benzoate, amyl acetate, isoamyl acetate, propyl acetate, butyl acetate, diethyl carbonate, methyl lactate, ethyl lactate, dibutyl maleate and the like.
  • organic solvents may be used individually by 1 type, or 2 or more types may be mixed and used for them.
  • Preferred examples of such organic solvents include propylene glycol monomethyl ether, n-hexanol, 2-ethyl-1-hexanol, and 2-butoxyethanol.
  • the FPD member-forming material is usually prepared by adding a silane compound (B) and, if necessary, a basic compound, an acidic compound or a metal chelate compound to an organic solvent (D) and mixing them well, then silica It can be prepared by dispersing particles (A), inorganic particles and thickener (C) in an organic solvent.
  • silica particles inorganic particles and thickener (C) in an organic solvent.
  • known ball mills, sand mills (bead mills, high shear bead mills), hogenizers, ultrasonic homogenizers, nanomizers, propeller mixers, high shear mixers, paint shakers, etc. depending on the dispersibility of silica particles (A) and inorganic particles.
  • a disperser and in particular, a highly dispersed fine particle dispersion ball mill and a sand mill (bead mill, high shear bead mill) can be suitably used.
  • the FPD member can be obtained by applying the FPD member forming material onto a substrate and forming a film thereon. Moreover, you may pattern a coating film in a defined shape according to the member to form.
  • a method of applying the FPD member forming material for example, a method of applying using a brush, roll coater, bar coater, flow coater, centrifugal coater, ultrasonic coater, (micro) gravure coater, dip coating method, flow coating, etc.
  • Methods such as a method, a spray method, a screen printing method, an electrodeposition method, and a vapor deposition method can be used.
  • the FPD member forming material of the present invention has fluidity
  • the FPD member forming material is applied to the surface of the glass substrate by a screen printing method or the like, and the coating film is dried, whereby the film forming material layer Can be formed.
  • the drying condition of the coating film is, for example, 40 to 150 ° C. for 1 to 60 minutes.
  • the dry film thickness is about 0.05 to 40 ⁇ m in the case of one coating, and the dry film thickness is 0.1 to in the case of two coatings.
  • a film having a thickness of about 80 ⁇ m can be formed.
  • one-time coating means that when the FPD member forming material is applied onto the substrate, the application operation of the FPD member forming material and the drying treatment of the coating film obtained thereby are defined as one cycle. This means that the coating is performed only once, and “twice coating” means that the coating operation of the FPD member forming material and the drying treatment of the coating film obtained thereby are defined as one cycle, and this cycle is repeated twice. Means that.
  • the film-forming material layer formed as described above is fired to decompose and remove organic substances (solvents and the like) and to be sintered.
  • the firing temperature is, for example, 400 to 650 ° C.
  • the firing time is, for example, 1 to 360 minutes.
  • isopropyl alcohol is injected into the sample cell and the background is measured.
  • silica particles (A) dispersed in isopropyl alcohol are injected into the sample cell so that the sample concentration falls within the appropriate concentration range of the apparatus. Measurement was selected, and the particle size distribution based on volume was measured under the conditions of a measurement time of 60 seconds and a measurement count of 1.
  • (3) Evaluation of transparency After coating the FPD member forming material on quartz glass so that the dry film thickness is 10 ⁇ m, it is dried at 80 ° C. for 20 minutes and then dried at 250 ° C. for 1 hour. A film was formed.
  • the transmittance of the obtained film was measured using a haze tester (touch panel type haze computer HZ-2S) manufactured by Suga Test Instruments Co., Ltd., and evaluated according to the following criteria.
  • Evaluation of film formability and heat resistance FPD member forming material is dried After coating on quartz glass so that the film thicknesses were 8 ⁇ m, 10 ⁇ m, 12 ⁇ m, 15 ⁇ m, and 30 ⁇ m, respectively, the film was dried at 80 ° C. for 20 minutes, and then dried at 250 ° C. for 1 hour to form a film.
  • the obtained film was baked at 500 ° C.
  • AAA No cracking even when the dry film thickness is 30 ⁇ m
  • AA No cracking even when the dry film thickness is 15 ⁇ m
  • silane compound (B1) a silane compound having a weight average molecular weight (Mw) of 5,000 (hereinafter referred to as “silane compound (B1)”).
  • silane compound (B2) a silane compound having a weight average molecular weight (Mw) of 1,000 (hereinafter referred to as “silane compound (B2)”).
  • Silane compound (B2) a silane compound having a weight average molecular weight of 1,000.
  • silane compound (B2) a silane compound having a weight average molecular weight of 1,000.
  • silane compound (B2) a silane compound having a weight average molecular weight (Mw) of 1,000 (hereinafter referred to as “silane compound (B2)”).
  • silane compound (B3) a silane compound having a weight average molecular weight (Mw) of 40,000 (hereinafter referred to as “silane compound (B3)”).
  • silane compound (B4) a silane compound having a weight average molecular weight (Mw) of 200 (hereinafter referred to as “silane compound (B4)”).
  • silane compound (B5) a silane compound having a weight average molecular weight (Mw) of 100,000 (hereinafter referred to as “silane compound (B5)”).
  • colloidal silica The properties of the colloidal silica used in the following examples and comparative examples are as follows.
  • Colloidal silica (A1) An isopropyl alcohol-dispersed silica sol containing 30% by mass of an SiO 2 component and having a silica particle diameter in the range of 0.05 to 0.25 ⁇ m.
  • Colloidal silica (A2) An isopropyl alcohol-dispersed silica sol containing 30% by mass of a SiO 2 component, wherein the silica particles have a particle size in the range of 0.01 to 0.03 ⁇ m.
  • Example 1 To 306 parts (95 parts of silica particles and 211 parts of propylene glycol monomethyl ether) obtained by replacing the solvent of colloidal silica (A1) by isopropyl alcohol with propylene glycol monomethyl ether, add 5 parts of silane compound (B1) and By stirring and mixing, the silane compound (B1) is dissolved in the solvent. Further, 3 parts of ethylcellulose is added as a thickener (C), and the mixture is sufficiently stirred to mix ethylcellulose in the solvent. Dissolved. Next, 189 parts of propylene glycol monoethyl ether was added, and the mixture was sufficiently stirred to prepare an FPD member forming material. The obtained FPD member forming material was evaluated for transparency, film forming property and heat resistance. The results are shown in Table 1.
  • Example 3 To 306 parts (95 parts of silica particles and 211 parts of propylene glycol monomethyl ether) obtained by replacing the solvent of colloidal silica (A1) by isopropyl alcohol with propylene glycol monomethyl ether, add 5 parts of silane compound (B1) and By stirring and mixing, the silane compound (B1) is dissolved in the solvent, and further 1 part of the copolymer (C1) is added as a thickener (C), and the mixture is sufficiently stirred and mixed. Copolymer (C1) was dissolved in a solvent. Next, 189 parts of propylene glycol monoethyl ether was added, and the mixture was sufficiently stirred to prepare an FPD member forming material. The obtained FPD member forming material was evaluated for transparency, film forming property and heat resistance. The results are shown in Table 1.
  • the silane compound (B1) is dissolved in a solvent, and further 10 parts of the copolymer (C1) is added as a thickener (C), and the mixture is sufficiently stirred and mixed to obtain the copolymer (C1). Was dissolved in a solvent. Next, 244 parts of solvent (D2) was added, and the mixture was sufficiently stirred to produce an FPD member forming material.
  • the obtained FPD member forming material was evaluated for transparency, film forming property and heat resistance. The results are shown in Table 1.
  • Example 5 Add 5 parts of silane compound (B1) to 306 parts (95 parts of silica particles and 211 parts of solvent (D2)) in which the solvent of colloidal silica (A1) is replaced with solvent (D2) from isopropyl alcohol.
  • the silane compound (B1) is dissolved in a solvent, and further, 3 parts of the copolymer (C2) is added as a thickener (C), and sufficiently stirred and mixed.
  • Copolymer (C2) was dissolved in a solvent.
  • 189 parts of solvent (D2) was added, and the mixture was sufficiently stirred to produce an FPD member forming material.
  • the obtained FPD member forming material was evaluated for transparency, film forming property and heat resistance. The results are shown in Table 1.
  • Example 6 Add 5 parts of silane compound (B1) to 306 parts (95 parts of silica particles and 211 parts of solvent (D2)) in which the solvent of colloidal silica (A1) is replaced with solvent (D2) from isopropyl alcohol.
  • the silane compound (B1) is dissolved in a solvent, and further, 10 parts of the copolymer (C2) is added as a thickener (C), and sufficiently stirred and mixed, Copolymer (C2) was dissolved in a solvent.
  • 189 parts of solvent (D2) was added, and the mixture was sufficiently stirred to produce an FPD member forming material.
  • the obtained FPD member forming material was evaluated for transparency, film forming property and heat resistance. The results are shown in Table 1.
  • Example 7 To 274 parts (silica particles 85 parts and solvent (D2) 189 parts) obtained by replacing the colloidal silica (A1) solvent from isopropyl alcohol with the solvent (D2), 15 parts of the silane compound (B1) are added sufficiently. By stirring and mixing, the silane compound (B1) is dissolved in the solvent, and further, 20 parts of the copolymer (C2) is added as a thickener (C), and sufficiently stirred and mixed. Copolymer (C2) was dissolved in a solvent. Next, 211 parts of a solvent (D2) was added, and the mixture was sufficiently stirred to produce an FPD member forming material. The obtained FPD member forming material was evaluated for transparency, film forming property and heat resistance. The results are shown in Table 1.
  • a silane compound (B1) is obtained by adding 5 parts of a silane compound (B1) to 306 parts of a solvent obtained by replacing the solvent of colloidal silica (A1) with isopropyl alcohol by propylene glycol monomethyl ether, and mixing with sufficient stirring. Was dissolved in a solvent. Next, 189 parts of propylene glycol monomethyl ether was added, and the mixture was sufficiently stirred to prepare an FPD member forming material. The obtained FPD member forming material was evaluated for transparency, film forming property and heat resistance. The results are shown in Table 1.
  • Example 8 To 306 parts (95 parts of silica particles and 211 parts of propylene glycol monomethyl ether) obtained by replacing the solvent of colloidal silica (A1) by isopropyl alcohol with propylene glycol monomethyl ether, add 5 parts of silane compound (B1) and By stirring and mixing, the silane compound (B1) is dissolved in the solvent. Further, 4.5 parts of ethyl cellulose is added as a thickener (C), and the mixture is sufficiently stirred and mixed to remove ethyl cellulose. Thus, an FPD member forming material was produced. The obtained FPD member forming material was evaluated for transparency, film forming property and heat resistance. The results are shown in Table 2.
  • Example 9 245 parts (76 parts of silica particles and 169 parts of solvent (D2)) obtained by substituting the solvent of colloidal silica (A1) with isopropyl alcohol for solvent (D2), and the solvent of colloidal silica (A2) from isopropyl alcohol to solvent ( 61 parts (19 parts of silica particles and 42 parts of solvent (D2)) were mixed with the one substituted with D2), and 5 parts of the silane compound (B1) was added to this mixture and mixed with sufficient stirring.
  • the silane compound (B1) is dissolved in a solvent, and 3.0 parts of ethyl cellulose is added as a thickener (C), and the mixture is sufficiently stirred to dissolve the ethyl cellulose in the solvent.
  • FPD member forming material was manufactured. The obtained FPD member forming material was evaluated for transparency, film forming property and heat resistance. The results are shown in Table 2.
  • Example 10 To 306 parts (95 parts of silica particles and 211 parts of propylene glycol monomethyl ether) obtained by replacing the solvent of colloidal silica (A1) by isopropyl alcohol with propylene glycol monomethyl ether, add 5 parts of silane compound (B1) and By stirring and mixing, the silane compound (B1) is dissolved in a solvent, and further 4.5 parts of the copolymer (C1) is added as a thickener (C) and mixed with sufficient stirring. Thus, ethyl cellulose was dissolved in a solvent, and thus an FPD member forming material was produced. The obtained FPD member forming material was evaluated for transparency, film forming property and heat resistance. The results are shown in Table 2.
  • Example 11 245 parts (76 parts of silica particles and 169 parts of solvent (D1)) obtained by replacing the solvent of colloidal silica (A1) with solvent (D1) from isopropyl alcohol, and the solvent of colloidal silica (A-2) from isopropyl alcohol 61 parts (19 parts of silica particles and 42 parts of solvent (D1)) mixed with the solvent (D1) are mixed, and 5 parts of the silane compound (B1) is added to this mixture and mixed with sufficient stirring. By dissolving the silane compound (B1) in the solvent, and further adding 3.0 parts of the copolymer (C1) as the thickener (C) and mixing with sufficient stirring, the copolymer is obtained. (C1) was dissolved in a solvent to produce an FPD member forming material. The obtained FPD member forming material was evaluated for transparency, film forming property and heat resistance. The results are shown in Table 2.
  • Example 12 To 306 parts (95 parts of silica particles and 211 parts of propylene glycol monomethyl ether) obtained by replacing the solvent of colloidal silica (A1) by isopropyl alcohol with propylene glycol monomethyl ether, add 5 parts of silane compound (B1) and By stirring and mixing, the silane compound (B1) is dissolved in a solvent, and further 4.5 parts of the copolymer (C2) is added as a thickener (C) and mixed with sufficient stirring. Thus, the copolymer (C2) was dissolved in a solvent, and thus an FPD member forming material was produced. The obtained FPD member forming material was evaluated for transparency, film forming property and heat resistance. The results are shown in Table 2.
  • Example 13 245 parts (76 parts of silica particles and 169 parts of solvent (D1)) obtained by replacing the solvent of colloidal silica (A1) with solvent (D1) from isopropyl alcohol, and the solvent of colloidal silica (A2) from isopropyl alcohol to solvent ( By mixing 61 parts (19 parts of silica particles and 42 parts of solvent (D1)) with the one substituted with D1), adding 5 parts of the silane compound (B1) to this mixture, and mixing with sufficient stirring The silane compound (B1) is dissolved in a solvent, and further 3.0 parts of the copolymer (C2) is added as a thickener (C), followed by thorough stirring and mixing. ) Was dissolved in a solvent to produce an FPD member forming material. The obtained FPD member forming material was evaluated for transparency, film forming property and heat resistance. The results are shown in Table 2.
  • Example 14 To 274 parts (silica particles 85 parts and propylene glycol monomethyl ether 189 parts) obtained by replacing the solvent of colloidal silica (A1) with isopropyl alcohol by propylene glycol monomethyl ether, add 15 parts of silane compound (B1) By stirring and mixing, the silane compound (B1) is dissolved in the solvent. Further, 10 parts of ethyl cellulose is added as a thickener (C), and the mixture is sufficiently stirred to mix ethyl cellulose into the solvent. It melt
  • Example 15 to 17 An FPD member forming material was manufactured in the same manner as in Example 1 except that the components shown in Table 3 were used as the components of the FPD member forming material. The obtained FPD member forming material was evaluated for transparency, film forming property and heat resistance. The results are shown in Table 3.

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Abstract

La présente invention concerne un matériau qui permet la production d'un élément d'écran plat qui n'entraîne aucune fissure et qui possède une haute résistance à la chaleur et une haute transparence. La présente invention concerne spécifiquement un matériau pour former un élément d'écran plat qui comprend : (A) des particules de silice ; (B) au moins un composé de silane qui possède un poids moléculaire moyen pondéral de 800 à 50000 et sélectionné parmi le groupe constitué d'un hydrolysat d'au moins un organosilane représenté par la formule (1) : R1nSi(OR2)4-n [où R1 représente un groupe organique univalent qui possède 1 à 8 atomes de carbone, à condition que, lorsque deux R1 ou plus sont présents, les R1 peuvent être identiques les uns aux autres ou différents les uns des autres ; les R2 représentent indépendamment un groupe alkyle qui possède 1 à 5 atomes de carbone ou un groupe acyle qui possède 1 à 6 atomes de carbone ; et n représente un nombre entier relatif de 0 à 3] et un produit de condensation de l'organosilane ; et (C) un agent épaississant.
PCT/JP2009/051958 2008-02-05 2009-02-05 Matériau pour la formation d'élément d'écran plat WO2009099141A1 (fr)

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JP2011241351A (ja) * 2010-05-21 2011-12-01 Jsr Corp 組成物およびフラットパネルディスプレイ部材形成材料
WO2012147250A1 (fr) * 2011-04-27 2012-11-01 パナソニック株式会社 Écran plasma
WO2013115367A1 (fr) * 2012-02-02 2013-08-08 日産化学工業株式会社 Composition filmogène présentant un indice de réfraction faible
WO2015005333A1 (fr) * 2013-07-11 2015-01-15 日産化学工業株式会社 Composition formant un film d'indice de réfraction élevé

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WO2001071761A1 (fr) * 2000-03-24 2001-09-27 Matsushita Electric Industrial Co., Ltd. Panneau d'affichage a plasma et son procede de fabrication
JP2003104755A (ja) * 2001-09-28 2003-04-09 Toray Ind Inc ペースト
JP2005108691A (ja) * 2003-09-30 2005-04-21 Korea Advanced Inst Of Sci Technol プラズマディスプレ−パネル用誘電体及びその製造方法

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WO2001071761A1 (fr) * 2000-03-24 2001-09-27 Matsushita Electric Industrial Co., Ltd. Panneau d'affichage a plasma et son procede de fabrication
JP2003104755A (ja) * 2001-09-28 2003-04-09 Toray Ind Inc ペースト
JP2005108691A (ja) * 2003-09-30 2005-04-21 Korea Advanced Inst Of Sci Technol プラズマディスプレ−パネル用誘電体及びその製造方法

Cited By (11)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2011241351A (ja) * 2010-05-21 2011-12-01 Jsr Corp 組成物およびフラットパネルディスプレイ部材形成材料
WO2012147250A1 (fr) * 2011-04-27 2012-11-01 パナソニック株式会社 Écran plasma
WO2013115367A1 (fr) * 2012-02-02 2013-08-08 日産化学工業株式会社 Composition filmogène présentant un indice de réfraction faible
CN104080869A (zh) * 2012-02-02 2014-10-01 日产化学工业株式会社 低折射率膜形成用组合物
KR20140120340A (ko) * 2012-02-02 2014-10-13 닛산 가가쿠 고교 가부시키 가이샤 저굴절율 막형성용 조성물
JPWO2013115367A1 (ja) * 2012-02-02 2015-05-11 日産化学工業株式会社 低屈折率膜形成用組成物
CN104080869B (zh) * 2012-02-02 2017-03-08 日产化学工业株式会社 低折射率膜形成用组合物
KR20200051853A (ko) * 2012-02-02 2020-05-13 닛산 가가쿠 가부시키가이샤 저굴절율 막형성용 조성물
KR102244973B1 (ko) * 2012-02-02 2021-04-27 닛산 가가쿠 가부시키가이샤 저굴절율 막형성용 조성물
KR102285627B1 (ko) * 2012-02-02 2021-08-04 닛산 가가쿠 가부시키가이샤 저굴절율 막형성용 조성물
WO2015005333A1 (fr) * 2013-07-11 2015-01-15 日産化学工業株式会社 Composition formant un film d'indice de réfraction élevé

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