JP2008026684A - Photosensitive paste - Google Patents

Abstract

<P>PROBLEM TO BE SOLVED: To provide a photosensitive paste capable of producing barrier ribs which are expected to have high mechanical strength and of which the pattern cross-sectional form is trapezoid. <P>SOLUTION: [1] The photosensitive paste contains (A) inorganic particles, (B) an alkali-soluble resin, (C) a crosslinking agent, (D) an acid generator, (E) an organic solvent and (F) 0.05-5 mass% of water based on the total amount of the photosensitive paste. There are also provided [2] barrier ribs for a plasma display obtained using the photosensitive paste [1] and [3] a member for a plasma display equipped with the barrier ribs [2]. <P>COPYRIGHT: (C)2008,JPO&INPIT

Description

  The present invention relates to a photosensitive paste. More specifically, the present invention relates to a photosensitive paste suitable for forming partition walls on a plasma display back plate.

  2. Description of the Related Art In recent years, high definition has been progressed in plasma displays, and accordingly, it is desired to improve the microfabrication technology for the partition pattern in the back plate of the plasma display. As a fine processing technique, for example, a lithography process using a photosensitive paste is applied.

  Examples of a conventional photosensitive paste for forming a partition wall include a photosensitive paste containing a photoacid generator, a crosslinking agent, and a novolac resin. The photosensitive paste is applied on a substrate, exposed, and developed. Then, a method is known in which pattern processing is performed and further baking is performed to form partition walls (see Patent Document 1).

JP 11-338144 A

When the photosensitive paste disclosed in Patent Document 1 is used and fine processing is performed by a lithography process, a pattern with a thin cross-sectional shape is easily obtained, and a partition obtained by firing such a pattern There was a concern that the mechanical strength would decrease. In order to obtain a practical mechanical strength of the partition wall, the pattern cross-sectional shape is preferably a trapezoidal shape, and the partition wall has been demanded. Moreover, the occurrence of such thinning is more remarkable when the pattern is a thick film.
An object of the present invention is to form a photosensitive paste that can easily produce a partition wall that is expected to have high mechanical strength because a thick film can be patterned with a single exposure and a cross-sectional shape becomes a trapezoidal pattern. It is to provide. Furthermore, another object of the present invention is to provide a partition using the photosensitive paste, a plasma display member including the partition, and a plasma display panel.

  As a result of intensive studies to find a photosensitive paste that can solve the above-mentioned problems, the present inventors have completed the present invention.

That is, the present invention includes [1] (A) inorganic particles (B) alkali-soluble resin (C) cross-linking agent (D) acid generator (E) organic solvent, and (F) water in the total amount of photosensitive paste. On the other hand, the photosensitive paste characterized by containing in 0.05-5 mass% is provided.

（式中、Ｑ₂、Ｑ₃は、それぞれ独立に式（４）で表される基であり、Ｑ₁は式（５）で示される基から選ばれる）

（式中、Ｔ₁は炭素数１〜６のアルキレン基、炭素数１〜６のアルキレンオキシアルキレン基またはフェニレン基を表す。ｍは０または１である。）

（式中、Ｔ₂〜Ｔ₇は、メチル基またはフェニル基を表す。Ｔ₈は酸素原子、メチレン基、エテニレン基、エチニレン基、フェニレン基、ナフタレンジイル基およびビフェニルジイル基からなる郡から選ばれる。）
［４］前記（Ｅ）が、２５℃における屈折率が１．４０〜１．８０の有機溶媒である、［１］〜［３］のいずれかに記載の感光性ペースト
［５］前記（Ａ）が、軟化点が４００℃〜６００℃である低融点ガラス粒子を含む無機粒子である、［１］〜［４］のいずれかに記載の感光性ペースト Furthermore, the present invention provides the following [2] to [5] as preferred embodiments according to the above [1].
[2] The content ratios of (A) to (E) to the photosensitive paste are (A) 20 to 95% by mass, (B) 2 to 30% by mass, and (C) 1 to 30% by mass, respectively. (D) 0.01 to 20% by mass and (E) 1 to 40% by mass of the photosensitive paste [3], wherein the (B) is a novolak resin and / or a part of the novolak resin An epoxy group-containing silicon compound in which the hydroxyl group is substituted with an OR ₃ group (wherein R ₃ is a monovalent organic group having 1 to 20 carbon atoms), and (C) is represented by the formula (3) The photosensitive paste according to [1] or [2]

(In the formula, Q ₂ and Q ₃ are each independently a group represented by the formula (4), and Q ₁ is selected from the group represented by the formula (5)).

(In the formula, T ₁ represents an alkylene group having 1 to 6 carbon atoms, an alkyleneoxyalkylene group having 1 to 6 carbon atoms, or a phenylene group. M is 0 or 1.)

(Wherein T _{2 to} T ₇ represent a methyl group or a phenyl group. T ₈ is selected from a group consisting of an oxygen atom, a methylene group, an ethenylene group, an ethynylene group, a phenylene group, a naphthalenediyl group, and a biphenyldiyl group. .)
[4] The photosensitive paste according to any one of [1] to [3], wherein (E) is an organic solvent having a refractive index of 1.40 to 1.80 at 25 ° C. [5] ) Is an inorganic particle containing low melting point glass particles having a softening point of 400 ° C. to 600 ° C. The photosensitive paste according to any one of [1] to [4]

The present invention also provides the following [6] to [8] using any of the photosensitive pastes described above.
[6] A plasma display panel comprising the plasma display panel barrier rib of [7] [6], which is manufactured using any one of the photosensitive pastes described above.
[8] A plasma display panel comprising the plasma display member according to [7].

Moreover, the following [9] suitable for manufacturing the partition of the plasma display panel is provided.
[9] Manufacturing method of partition for plasma display panel comprising the following steps (a) Step of forming a coating film by applying any of the above photosensitive pastes on a substrate (b) Heating the coating film after coating Step (c) Step of exposing the coating film obtained in the above (b) (d) Step of heating the coated film after exposure (e) Step of developing the coating film (f) After development, the substrate is 450 The process of baking at a temperature of from ℃ to 600 ℃

According to the photosensitive paste of the present invention, it is possible to form a pattern with a single exposure even with a thick film exceeding 50 μm, and it is possible to perform pattern processing with a trapezoidal cross-sectional shape expected to have high mechanical strength. . A partition wall obtained by using such pattern processing can be obtained with excellent mechanical strength.
Moreover, the said partition can be used suitably as a backplate for plasma displays, Furthermore, a plasma display panel can be provided from this backplate.

  Hereinafter, preferred embodiments of the present invention will be described.

The photosensitive paste of the present invention is
(A) Inorganic particles (B) Alkali-soluble resin (C) Crosslinker (D) Acid generator (E) Organic solvent (F) A photosensitive paste comprising water, (F) Water content The total amount of the photosensitive paste is 0.05 to 5% by mass. (F) As content of water, Preferably it is the range of 0.1-4 mass%, More preferably, it is the range of 0.1-3 mass%. When this content is less than 0.05% by mass, thinning is likely to occur in the cross-sectional shape of the pattern. On the other hand, when it exceeds 5% by mass, the above (E) and water are likely to be phase-separated. From an adhesive paste, it tends to be difficult to obtain a uniform coating film when applied to a substrate.

In order to control the content of (F) water in the photosensitive paste, when mixing the above (A) to (F), a method of measuring and mixing so that (F) is in the above range. Alternatively, the above (A) to (E) are mixed in advance to obtain a mixture, and the moisture content of the mixture is measured using a car fisher moisture meter or the like, and then (F) is within the above range. A method of adding water later may be used.
When preparing the photosensitive paste in this way, as (F) above, water having a resistivity of 17 MΩ · cm or more at 25 ° C. is usually used from ion-exchanged water, pure water or ultrapure water. Is preferred. Water exhibiting such a resistivity can be easily obtained by using a commercially available pure water production apparatus.

Next, (A) inorganic particles will be described.
The relative dielectric constant of (A) is preferably in the range of 4.0 to 9.5 at a measurement temperature of 20 ° C., more preferably 4.0 to 9.0. A partition obtained using a photosensitive paste containing (A) having a relative dielectric constant in the above range is preferable because reactive power when driven as a plasma display panel is reduced. Here, the relative dielectric constant can be measured using a commercially available bridge-type dielectric constant measuring device (for example, model number TR-10C manufactured by Ando Electric Co., Ltd. can be mentioned).

  The refractive index of (A) is preferably in the range of 1.40 to 2.50, more preferably in the range of 1.43 to 2.20, particularly preferably 1 at a measurement temperature of 25 ° C. The range is from .43 to 1.80. When the refractive index of (A) is in the above range, light scattering is small during exposure, which tends to form a good pattern, which is preferable. The refractive index can be measured using a commercially available prism refractive index measuring device (for example, model number GP1-P manufactured by OPTEC).

  Furthermore, the volume average particle diameter of (A) is preferably 0.01 to 40 μm, more preferably 0.1 to 10 μm, and particularly preferably 1 to 8 μm at a measurement temperature of 25 ° C. When the average particle size is in the above range, the amount of (A) can be increased when adjusting the photosensitive paste, and the pattern obtained from such a photosensitive paste has a shrinkage during firing. This is preferable because the amount of light is small, and since light scattering during exposure is small, a good pattern tends to be formed. The volume average particle diameter can be measured using a commercially available light scattering particle diameter measuring apparatus (for example, model number DLS-7000 manufactured by Otsuka Electronics Co., Ltd.).

  In the photosensitive paste of the present invention, inorganic particles having different volume average particle diameters may be mixed at an arbitrary ratio and used as (A).

  The shape of the inorganic particles is not particularly limited and may be crushed or spherical, but is preferably spherical.

  Examples of (A) include silica particles derived from colloidal silica, silica particles such as aerosil and silica gel, low-melting glass particles having a softening point of 400 ° C to 600 ° C, or glass particles having a softening temperature of 601 ° C or higher. Or mixtures thereof. In particular, a photosensitive paste containing inorganic particles containing low-melting glass particles as (A) is preferable because the obtained partition walls have high strength. Here, examples of the low melting point glass particles include zinc oxide glass, tin oxide phosphate glass, bismuth oxide glass, and lead glass.

  The addition ratio of (A) used in the photosensitive paste of the present invention is preferably 20 to 95% by mass and more preferably 40 to 95% by mass with respect to the total amount of the photosensitive paste.

  When the addition ratio of (A) is in the above range, film shrinkage during firing is reduced, and further, it is difficult to peel off from the substrate, and light scattering during exposure tends to be reduced, so that a favorable pattern can be formed. Is preferable.

Next, (B) the alkali-soluble resin will be described.
Here, the notation of alkali-soluble represents that it can be dissolved in either an alkaline aqueous solution, an organic solvent exhibiting alkalinity, or an organic solvent-water mixed solution exhibiting alkalinity. Examples of the alkali-soluble group that exhibits such alkali-solubility include a carboxyl group (—COOH), a phenolic hydroxyl group, a phosphonic acid group (—PO ₃ H ₂ ), a sulfonic acid group (—SO ₃ H), and a sulfonic imide group (— SO ₂ NHSO ₂ —) is at least one acid group selected from the group consisting of a carboxylic acid anhydride group, a group in which a phenolic hydroxyl group is protected by esterification or etherification, and the like. Mention may be made of groups which are converted into groups. As the resin having an alkali-soluble group, known resins can be used. For example, novolak resin and derivatives thereof, styrene-maleic anhydride copolymer, polyvinylhydroxybenzoate and derivatives thereof, polyhydroxystyrene and derivatives thereof. Derivatives, carboxyl group-containing acrylic resins and derivatives thereof, polystyrene sulfonic acid and derivatives thereof, and the like.

（式中、ｎは０以上２以下の整数を表わす。Ｒ₁は炭素数１〜２０の一価の有機基を表し、ｎが２の場合、２つあるＲ₁は同一あるいは異なっていてもよい。）

（式中、Ｒ₂は、水素原子または炭素数１〜２０の一価の有機基を表す）
（ｂ）ノボラック樹脂（ａ）のフェノール性水酸基の一部をＯＲ₃基に置換した樹脂（ここで、Ｒ₃は炭素数１〜２０の一価の有機基である） In particular, among the examples of the alkali-soluble resin, (B) applied to the present invention includes a novolak resin having a phenolic hydroxyl group, or a novolak in which a part of the phenolic hydroxyl group of the novolak resin is protected by etherification. Resin derivatives are preferred.
Specifically, it is preferable to use one or more selected from (a) and (b) below as (B).

(A) A novolak resin obtained by polycondensation of a phenol compound represented by formula (1) and an aldehyde compound represented by formula (2)

(In the formula, n represents an integer of 0 or more and 2 or less. R ₁ represents a monovalent organic group having 1 to 20 carbon atoms, and when n is 2, two R _{1 s} may be the same or different. Good.)

(Wherein R ₂ represents a hydrogen atom or a monovalent organic group having 1 to 20 carbon atoms)
(B) A resin in which a part of the phenolic hydroxyl group of the novolak resin (a) is substituted with an OR ₃ group (where R ₃ is a monovalent organic group having 1 to 20 carbon atoms)

The (a) is a novolak resin obtained by polycondensation of the phenol compound represented by the above formula (1) and the aldehyde compound represented by the formula (2), where R ₁ in the formula (1) is carbon. The monovalent organic group of number 1-20 is represented. The monovalent organic group having 1 to 20 carbon atoms may be linear, branched or cyclic, and examples thereof include a linear aliphatic hydrocarbon group having 1 to 20 carbon atoms and 3 to 20 carbon atoms. A branched aliphatic hydrocarbon group, a cyclic aliphatic hydrocarbon group having 3 to 20 carbon atoms, an aromatic hydrocarbon group having 6 to 20 carbon atoms, and the like. The aromatic hydrocarbon group may be substituted with an alkyl group, an alkenyl group or the like.

  Among these, a straight hydrocarbon group having 1 to 6 carbon atoms, a branched hydrocarbon group having 3 to 6 carbon atoms, a cyclic hydrocarbon group having 3 to 6 carbon atoms, and an aromatic carbon atom having 6 to 20 carbon atoms. A hydrogen group is preferred.

  Examples of the linear aliphatic hydrocarbon group having 1 to 20 carbon atoms include methyl, ethyl, propyl, butyl, pentyl, hexyl, heptyl, octyl, nonyl, decyl, and dodecyl. Group, undecyl group, tridecyl group, tetradecyl group, pentadecyl group, hexadecyl group, heptadecyl group, octadecyl group, nonadecyl group, icosyl group and the like, in particular, methyl group, ethyl group, propyl group, butyl group, pentyl group, A hexyl group is preferred.

  Examples of the branched aliphatic hydrocarbon group having 3 to 20 carbon atoms include isopropyl group, isobutyl group, tertiary butyl group, tertiary octyl group, and the like, and isopropyl group and isobutyl group are particularly preferable.

  Examples of the cycloaliphatic hydrocarbon group having 3 to 20 carbon atoms include a cyclopropyl group, a cyclobutyl group, a cyclopentyl group, a cyclohexyl group, a cycloheptyl group, a cyclooctyl group, and the like. In particular, a cyclopentyl group and a cyclohexyl group are exemplified. preferable.

  As a C6-C20 aromatic hydrocarbon group, the sum total of the carbon number which comprises group is a thing of 6-20. Here, examples of the substituent in the aromatic hydrocarbon group include alkyl groups such as methyl group, ethyl group, propyl group, and butyl group, alkenyl groups such as allyl group and vinyl group, alkenyloxy groups such as allyloxy group, Examples thereof include alkynyl groups such as ethynyl group and alkynyloxy groups such as ethynyloxy group.

  Specific examples of the aromatic hydrocarbon group having 6 to 20 carbon atoms include phenyl group, naphthyl group, anthryl group, tolyl group, xylyl group, trimethylphenyl group, ethylphenyl group, diethylphenyl group, triethylphenyl group, propyl A phenyl group, a butylphenyl group, a methyl naphthyl group, a dimethyl naphthyl group, a trimethyl naphthyl group, a vinyl naphthyl group, a methyl anthryl group, an ethyl anthryl group and the like can be mentioned, and a phenyl group, a tolyl group and a xylyl group are particularly preferable.

The substitution position of R ₁ in the formula (1) is preferably _one in which at least two positions are not substituted from the phenol hydroxyl group at the 2-position, 4-position, and 6-position. Specifically, phenol (hydroxybenzene), o-cresol, m-cresol, p-cresol, o-ethylphenol, m-ethylphenol, p-ethylphenol, o-propylphenol, m-propylphenol, p-propylphenol, o-isopropylphenol, m-isopropyl Phenol, p-isopropylphenol, o-tertiarybutylphenol, m-tertiarybutylphenol, o-hexylphenol, m-hexylphenol, o-decylphenol, m-decylphenol, o-dodecylphenol, m-dodecylphenol, o -Hexade Silphenol, m-hexadecylphenol, o-icosylphenol, m-icosylphenol, o-cyclopentylphenol, m-cyclopentylphenol, o-cyclohexylphenol, m-cyclohexylphenol, o-cycloheptylphenol, m-cyclo Heptylphenol, o-phenylphenol, m-phenylphenol, o-toluylphenol, m-toluylphenol, o-naphthylphenol, m-naphthylphenol,
2,5-xylenol, 2,3-xylenol, 3,5-xylenol, 2-ethyl-5-methylphenol, 2-ethyl-3-methylphenol, 3-ethyl-5-methylphenol, 2-isopropyl-5 -Methylphenol, 2-isopropyl-3-methylphenol, 3-isopropyl-5-methylphenol, 2-tertiarybutyl-5-methylphenol, 2-tertiarybutyl-3-methylphenol, 3-tertiarybutyl- 5-methylphenol, 2-hexyl-5-methylphenol, 2-hexyl-3-methylphenol, 3-hexyl-5-methylphenol, 2-cyclohexyl-5-methylphenol, 2-cyclohexyl-3-methylphenol, 3-cyclohexyl-5-methylphenol, 2-phenyl Nyl-5-methylphenol, 2-phenyl-3-methylphenol, 3-phenyl-5-methylphenol, 2-naphthyl-5-methylphenol, 2-naphthyl-3-methylphenol, 3-naphthyl-5-methyl Phenol, 2,5-diethylphenol, 2,3-diethylphenol, 3,5-diethylphenol, 2,5-dipropylphenol, 2,3-dipropylphenol, 3,5-dipropylphenol, 2,5 -Biscyclohexylphenol, 2,3-biscyclohexylphenol, 3,5-biscyclohexylphenol, 2,5-diphenylphenol, 2,3-diphenylphenol, 3,5-diphenylphenol and the like.
In particular, phenol (hydroxybenzene), o-cresol, m-cresol, p-cresol, 2,5-xylenol, 3,5-xylenol, 2,3-xylenol, 2-butylphenol, 2-isobutylphenol, 2-cyclohexyl Phenol and 2-phenylphenol are preferable, and phenol (hydroxybenzene), o-cresol, m-cresol, and p-cresol are particularly preferable.

R ₂ in Formula (2) is selected from a hydrogen atom or a monovalent organic group having 1 to 20 carbon atoms, and examples of the monovalent organic group include those equivalent to R ₁ described above. Specific examples of the aldehyde compound represented by the formula (2) include formaldehyde, acetaldehyde, propanal, butanal, hexanal, octanal, decanal, dodecanal, hexadecanal, icosanal, 2-methylpropanal, 2-methylbutanal. 2-ethylbutanal, 2,2-dimethylpropanal, acrolein, 2-butenal, 2-hexenal, 2-octenal, acetylenic aldehyde, 2-butynal, 2-hexinal, 2-octynal, cycloheptylcarbalaldehyde, Examples include cyclohexyl carbaldehyde, benzaldehyde, 1-naphthyl aldehyde, 2-naphthyl aldehyde, and styryl aldehyde. As the aldehyde compound, a depolymerizable polymer precursor can be used, and the aldehyde group may be protected with an acetal group or a hemiacetal group.

  Among the aldehyde compounds represented by the formula (2), formaldehyde and acetaldehyde are particularly preferable, and formaldehyde is particularly preferable. As formaldehyde, paraformaldehyde which is a depolymerizable polymer or formalin which is an aqueous solution can also be used.

  The polycondensation method of the compound represented by the formula (1) and the aldehyde compound represented by the formula (2) is not particularly limited. For example, an acid catalyst or an alkali catalyst is used in the presence or absence of a reaction solvent. Can be achieved. The reaction temperature is 0 to 200 ° C., preferably 50 to 150 ° C., and the reaction time is 0.1 to 30 hours, preferably 1 to 20 hours. Examples of the acid catalyst include sulfuric acid, hydrochloric acid, nitric acid, phosphoric acid, acetic acid, oxalic acid, malonic acid, and toluenesulfonic acid. Examples of the alkali catalyst include sodium hydroxide, potassium hydroxide, cesium hydroxide, sodium carbonate, and carbonic acid. Examples include sodium hydride, ammonia, tetramethylammonium hydroxide, triethylamine, morpholine, and pyridine.

  Reaction solvents used for polycondensation include alcohols such as methanol, ethanol, isopropanol, and tertiary butyl alcohol; ketones such as methyl ethyl ketone, methyl isobutyl ketone, methyl hexyl ketone, methyl heptyl ketone, and cyclohexyl ketone; propyl acetate, butyl acetate , Esters such as isobutyl acetate, methyl propionate, ethyl lactate, propylene glycol acetate; ethers such as dibutyl ether, tetrahydrofuran, tetrahydropyran, dioxane; aromatic hydrocarbons such as benzene, toluene, xylene; dichloromethane, chloroform, Halogenated hydrocarbons such as carbon tetrachloride and bromoform; hydrocarbons such as hexane, heptane, decane, and petroleum ether can be used. It can be used as a mixture of the above. In addition, water may coexist in the reaction system, and in the case of a solvent that is incompatible with water, a reaction solvent separated into two layers may be used. Water may be removed by distillation dehydration or the like.

  In the above polycondensation method, ketones, esters or aromatic hydrocarbons are used as a reaction solvent, organic acids such as acetic acid, oxalic acid, malonic acid, toluenesulfonic acid or ammonia, tetramethylammonium hydroxide, It is preferable to use an alkali such as triethylamine as a catalyst. The catalyst may or may not dissolve in the reaction solvent used.

In the above (b), a part of the phenolic hydroxyl group of the novolak resin (a) obtained as described above is substituted with an OR ₃ group. Here, R ₃ is a monovalent organic group having 1 to 20 carbon atoms, and examples equivalent to R ₁ or R ₂ can be given.

Examples of the reaction for replacing the phenolic hydroxyl group with an OR ₃ group include strong alkalis such as sodium hydroxide, potassium hydroxide, metallic sodium, metallic lithium, metallic potassium, n-butyllithium, sodium naphthalate, and sodium methoxide. It can be used by converting the phenolic hydroxyl group into a metal phenolate group and reacting the compound represented by the formula (6).

（式中、Ｒ₃は前記と同等の定義である。Ｔはフッ素原子、塩素原子、臭素原子、ヨウ素原子、メシル基およびトシル基からなる群から選ばれる。）
式（６）で示される化合物は、使用するノボラック樹脂（ａ）のフェノール性水酸基１モル当量に対して、０．９９モル当量以下、好ましくは０．８モル当量以下、特に好ましくは０．５モル当量以下を使用する。
ここで、使用するノボラック樹脂（ａ）中のフェノール性水酸基のモル当量は、アルカリ滴定法を用いて求めることができる。

(In the formula, R ₃ has the same definition as above. T is selected from the group consisting of a fluorine atom, a chlorine atom, a bromine atom, an iodine atom, a mesyl group, and a tosyl group.)
The compound represented by the formula (6) is 0.99 molar equivalent or less, preferably 0.8 molar equivalent or less, particularly preferably 0.5 molar equivalent to 1 molar equivalent of the phenolic hydroxyl group of the novolak resin (a) to be used. Use molar equivalents or less.
Here, the molar equivalent of the phenolic hydroxyl group in the novolak resin (a) to be used can be determined using an alkali titration method.

  Specific examples of the compound represented by the formula (6) are methyl fluoride, ethyl fluoride, decyl fluoride, hexyl fluoride, octyl fluoride, dodecyl fluoride, hexadecyl fluoride, icosyl fluoride, methyl chloride, ethyl chloride. , Decyl chloride, hexyl chloride, octyl chloride, dodecyl chloride, hexadecyl chloride, icosyl chloride, methyl bromide, ethyl bromide, decyl bromide, hexyl bromide, octyl bromide, dodecyl bromide, hexadecyl bromide, icosyl bromide , Benzyl bromide, methyl iodide, ethyl iodide, decyl iodide, hexyl iodide, octyl iodide, dodecyl iodide, hexadecyl iodide, icosyl iodide, benzyl iodide, methyl ethyl sulfonate, methyl butyl sulfonate , Methyl octyl sulfonate, methyl decyl sulfonate, toluyl ethyl sulfonate, buty Acid toluyl, octyl sulfonic acid toluyl, cited toluic decyl sulfonate and the like, methyl bromide, ethyl bromide, methyl iodide, ethyl iodide are preferred.

  Examples of the reaction solvent include alcohols such as methanol, ethanol, isopropanol, and tertiary butyl alcohol; ketones such as methyl ethyl ketone, methyl isobutyl ketone, methyl hexyl ketone, methyl heptyl ketone, and cyclohexyl ketone; dibutyl ether, tetrahydrofuran, tetrahydropyran, and dioxane. Ethers such as benzene, toluene, xylene, etc .; hydrocarbons such as dichloromethane, chloroform, carbon tetrachloride, bromoform; hydrocarbons such as hexane, heptane, decane, petroleum ether, etc. These may be used alone or in combination of two or more. In particular, ethers, aromatic hydrocarbons or halogenated hydrocarbons are preferred. In the reaction, water may coexist as long as the reactant used is not deactivated, but a dehydrated solvent having a water content of 100 ppm or less is preferred. The reaction temperature is 0.1 to 20 hours, preferably 1 to 10 hours, and the reaction temperature is −60 to 100 ° C., preferably −20 to 50 ° C.

In particular, (B) of the present invention is particularly preferably a phenol novolak resin or a cresol novolak resin obtained by polymerizing formaldehyde with a compound in which R ₁ in formula (1) is a hydrogen atom or a methyl group. Phenol novolac resins or cresol novolac resins can be preferably used because of high dissolution contrast. Moreover, the addition ratio of (B) used for the photosensitive paste of this invention becomes like this. Preferably it is 2-30 mass% with respect to the photosensitive paste total amount, More preferably, it is 3-20 mass%.

  (A) or (b) obtained as described above is the catalyst or catalyst residue used in the polycondensation reaction or substitution reaction, the phenol compound represented by the unreacted formula (1), the unreacted formula (2) It is preferable to remove the aldehyde compound represented by) or the unreacted compound represented by the formula (6) by a known method. The reaction solvent used in the above polycondensation reaction or the above substitution reaction can also be removed by a known method. However, when a solvent applicable to (E) described later is used as a reaction solvent, it is not removed. A solution in which an alkali-soluble resin is dissolved may be used for preparing the photosensitive paste of the present invention.

  The polystyrene-converted weight average molecular weight of the alkali-soluble resin (B) by gel permeation chromatography (hereinafter referred to as “GPC method”) is preferably 350 to 30,000, more preferably 350 to 10,000. It is. When the weight average molecular weight is in the above range, the curability of the exposed area tends to be high, the solubility of the unexposed area tends to be high, and the pattern formation characteristics tend to be favorable, which is preferable.

（式中、Ｑ₂、Ｑ₃は、それぞれ独立に式（４）で表される基であり、Ｑ₁は式（５ａ）または式（５ｂ）で示される基である。）

（式中、Ｔ₁は炭素数１〜６のアルキレン基、炭素数１〜６のアルキレンオキシアルキレン基またはフェニレン基を表す。ｍは０または１である。）

（式中、Ｔ₂〜Ｔ₇は、メチル基またはフェニル基を表す。Ｔ₈は酸素原子、メチレン基、エテニレン基、エチニレン基、フェニレン基、ナフタレンジイル基およびビフェニルジイル基からなる群から選ばれる。） Next, the crosslinking agent (C) will be described.
Examples of the crosslinking agent (C) include an epoxy-containing silicon compound represented by the formula (3).

(Wherein Q ₂ and Q ₃ are each independently a group represented by the formula (4), and Q ₁ is a group represented by the formula (5a) or the formula (5b)).

(In the formula, T ₁ represents an alkylene group having 1 to 6 carbon atoms, an alkyleneoxyalkylene group having 1 to 6 carbon atoms, or a phenylene group. M is 0 or 1.)

(Wherein T _{2 to} T ₇ represent a methyl group or a phenyl group. T ₈ is selected from the group consisting of an oxygen atom, a methylene group, an ethenylene group, an ethynylene group, a phenylene group, a naphthalenediyl group, and a biphenyldiyl group. .)

Here, Q ₂ and Q ₃ each independently represent a group having an epoxy group or an oxetane group represented by the formula (4). Here, when T ₁ is an alkylene group, examples thereof include glycidyl group, 1,2-epoxybutyl group, 1,2-epoxyhexyl group, and when alkylene group is alkyleneoxyalkylene group, glycidyloxyethyl group, glycidyloxy Examples thereof include a propyl group, a glycidyloxybutyl group, a 1,3-epoxybutyl group, and a 1,3-epoxyhexyl group. When T ₁ is a phenylene group, 1,2-epoxyethylphenyl group, 1,3-epoxypropylphenyl group and the like can be mentioned. In particular, the case where T ₁ is an alkyleneoxyalkylene group is preferable since it is simple in production, and a glycidyloxypropyl group is particularly preferable.
Q ₁ is a divalent group having one or two silicon atoms represented by the formula (5a) or (5b), and is a dimethylsilanediyl group, diphenylsilanediyl group, 1,1,3,3 -Tetramethyldisiloxanediyl group, 1,1,3,3-tetraphenyldisiloxanediyl group, 1,1,3,3-tetramethyldisilamethylenediyl group, phenylenebis (dimethylsilylene) group, etc. 1,1,3,3-tetramethyldisiloxanediyl group is particularly preferred.
As (C), 1,3-di (3′-glycidyloxypropyl) -1,1,3,3, -tetramethyldisiloxane is particularly preferable. 1,3-di (3′-glycidyloxypropyl) -1,1,3,3, -tetramethyldisiloxane is commercially available for use as an epoxy resin modifier and is readily available. is there.

  The addition ratio of (C) used in the photosensitive paste of the present invention is preferably 1 to 30% by mass and more preferably 1 to 20% by mass with respect to the total amount of the photosensitive paste.

Next, (D) the acid generator will be described.
Examples of (D) include a photoacid generator and a photocationic polymerization initiator.

  Examples of the photoacid generator include [cyclohexyl- (2-cyclohexanonyl) -methyl] sulfonium trifluoromethanesulfonate, bis (p-tolylsulfonyl) diazomethane, bis (cyclohexylsulfonyl) diazomethane, and tertiary butylcarbonylmethyl. -Tetrahydrothiophenium trifluoromethanesulfonate etc. are mentioned. As the photoacid generator, in addition to the above, compounds described in JP-A-11-202495 can also be used.

  Examples of the photocationic polymerization initiator include iodonium salts, sulfonium salts, phosphate salts, and antimonate salts. Specifically, Rhodesyl Photoinitiator 2074 (manufactured by Rodel), Adekaoptomer SP-150, Adekaoptomer SP-152, Adekaoptomer SP-170, Adekaoptomer SP-172 (all Asahi Denka Kogyo Co., Ltd.) Etc.). In addition to the above, compounds described in JP-A-9-118663 can also be used.

  The content of (D) with respect to the photosensitive paste of the present invention is preferably 0.01 to 20% by mass, more preferably 0.05 to 10% by mass, based on the total amount of the paste.

  When the content of (D) is in the above range, there is a tendency that a pattern can be formed with good productivity, which is preferable.

Next, (E) will be described.
(E) is preferably an organic solvent having a refractive index of 1.40 to 1.80 at 25 ° C. When the photosensitive paste contains two or more kinds of organic solvents, at least one organic solvent is Any organic solvent that satisfies the above refractive index may be used. In particular, it is preferable that all of the organic solvents applied to the photosensitive paste satisfy the above refractive index. As this refractive index, the range of 1.41-1.70 is more preferable, and the range whose refractive index is 1.42-1.60 is especially preferable. When the refractive index of (E) is in the above range, the transparency of the photosensitive paste after film formation tends to be high, which is preferable. The refractive index of the organic solvent can be measured at a measurement temperature of 25 ° C. using a refractometer (for example, RA-520N manufactured by Kyoto Electronics Industry Co., Ltd.). The refractive index should be selected from the values described in the literature, for example, revised 4th edition, Chemical Handbook, Basics II, pages 514-520 (edited by the Chemical Society of Japan, Maruzen Co., Ltd., issued on September 30, 1993). You can also.

  Here, examples of the organic solvent having a refractive index of 1.40 to 1.80 include propylene glycol monobutyl ether (refractive index 1.42), polypropylene glycol dibenzoate (refractive index 1.52), 2-heptanone ( Refractive index 1.41), propylene glycol methyl ether acetate (refractive index 1.40), gamma-butyrolactone (refractive index 1.44), 1,2-propanediol dibenzoate (refractive index 1.54), ethylene glycol di Examples thereof include acetate (refractive index: 1.42).

  As content of (E) in the photosensitive paste of this invention, it is 1-40 mass% normally with respect to the photosensitive paste total amount, Preferably it is 3-30 mass%, More preferably, it is 5-20 mass. %.

  Furthermore, you may add additives, such as a light absorber, a photosensitizer, a plasticizer, a dispersing agent, a precipitation inhibitor, and surfactant, to the photosensitive paste of this invention as needed.

Next, a method for producing a partition for a plasma display by performing pattern processing using the photosensitive paste of the present invention will be described with an example, but the present invention is not limited to this method.
As a suitable example in this manufacturing method, the manufacturing method which has the process shown to the following (a)-(e) is mentioned.
(A) The process of apply | coating the photosensitive paste in any one of the above on a board | substrate, and forming a coating film (b) The process of heating the coating film after application | coating (c) The coating film obtained by said (b) (D) Step of heating the coated film after exposure (e) Step of developing the coated film (f) Step of baking the substrate at a temperature of 450 ° C. to 600 ° C. after development

  First, (a) will be described. On the substrate, the photosensitive paste of the present invention is applied over the entire surface or partially. As a coating method, for example, a bar coater, a roll coater, a die coater, a screen printing method or the like can be used. The coating thickness can be adjusted by selecting the number of coatings and the viscosity of the paste, and is usually about 5 to 500 μm.

  When applying the photosensitive paste on the substrate, the surface of the substrate may be treated with a surface treatment liquid in order to further improve the adhesion between the substrate and the coating film.

  Examples of the surface treatment liquid include silane coupling agents such as glycidyloxypropyltriethoxysilane, glycidyloxypropyltrimethoxysilane, and oxetanyloxypropyltriethoxysilane. As the silane coupling agent, it is preferable to use a silane coupling agent diluted to a concentration of 0.1 to 5% with an organic solvent such as ethylene glycol monomethyl ether, methyl alcohol, ethyl alcohol, propyl alcohol, or butyl alcohol.

  Examples of the surface treatment method include a method in which a surface treatment liquid is uniformly applied on a substrate with a spinner or the like and then dried at 80 to 140 ° C. for 5 to 60 minutes. As a drying method, it is preferable to use a hot plate or a far-infrared oven.

  As described above, if necessary, a photosensitive paste is applied to the surface-treated substrate, and (b) is usually dried at 80 to 130 ° C. for 5 to 100 minutes using a far infrared oven or the like.

  After drying, (c) exposure is performed using an exposure apparatus. Examples of the exposure apparatus include a proximity exposure machine.

  When exposing a large area, a large area can be exposed with an exposure machine having a small exposure area by applying a photosensitive paste on a substrate and then performing exposure while moving the photosensitive paste. Exposure refers to drawing a pattern by irradiating a photosensitive paste coating film with ionizing radiation through a mask pattern to be created. Examples of ionizing radiation include ultraviolet rays, electron beams, X-rays, and visible light. Near infrared light can be used.

  The amount of irradiation in the exposure can be optimized as appropriate depending on the type of exposure source used or the type of (C) used in the photosensitive paste. As long as it does not interfere with this, there is no problem.

Particularly preferably, using the wavelength 365nm of light source using a high pressure mercury lamp as an exposure source, the temperature is achieved at room temperature (25 ± 5 ℃) under exposure amount ^{100mJ / cm 2 ~2000mJ / cm 2} .

  After the exposure, (d) using a far infrared oven or the like, drying is usually performed at 80 to 150 ° C. for 3 to 60 minutes. Next, (e) development is performed. Development is usually carried out by a dipping method, a spray method, a brush method or the like.

  Examples of the developer include aqueous alkali solutions such as tetramethylammonium hydroxide, monoethanolamine, diethanolamine, sodium hydroxide, sodium carbonate, potassium hydroxide, and potassium carbonate.

  The alkali concentration in the aqueous solution is preferably 0.05 to 5% by mass, more preferably 0.1 to 5% by mass. When the alkali concentration is in the above range, the removability of the portion to be developed and removed is good, and the pattern to be left is less likely to be peeled off or eroded, which is preferable.

  The temperature during development is preferably 15 to 50 ° C. in terms of process control.

  After the pattern is formed as described above, the partition walls can be manufactured by (f) firing in a firing furnace. The firing atmosphere and firing temperature vary depending on the type of photosensitive paste and substrate, but can be usually fired at 450 to 600 ° C. in an atmosphere such as air or nitrogen. As the firing furnace, a batch-type firing furnace or a belt-type continuous firing furnace can be used.

  In particular, when a partition wall is produced on a glass substrate, firing is usually performed at a temperature of 450 to 600 ° C. for 10 to 60 minutes.

  A coat layer may be formed on the surface of the partition wall obtained as described above. The coating layer is formed by applying and drying a coating agent such as a paste agent or a ceramic coating agent composed of low melting point glass particles and a binder resin, and baking it to form on the surface of the partition wall, or after forming the pattern, the coating agent After coating, the coating layer may be formed on the surface of the partition simultaneously with the formation of the partition by baking.

  Examples of the low melting point glass particles include the same examples as described above.

  Examples of the binder resin include butyral resin, polyvinyl alcohol, acrylic resin, and poly α-methylstyrene.

  As the ceramic coating agent, an aqueous metal salt coating agent, an alkoxy metal salt coating agent, or the like can be used. Specifically, as the aqueous metal salt coating agent, MS-1700, an alkoxy metal salt coating agent is used. Examples of the agent include G-301 and G-401 (both manufactured by Nippon Ceramic Co., Ltd.).

  The firing temperature of the coating layer is usually about 250 to 600 ° C. when a paste agent composed of low melting glass particles and a binder resin is used, and is usually room temperature to 500 ° C. when a ceramic coating agent is used.

  By manufacturing the diaphragm including the exposure, development, and baking described above, the cross-sectional shape (profile) has been conventionally reduced in contrast to a thick-walled diaphragm whose profile (profile) is likely to be a shape having a thin shape (FIG. 1). A partition wall (FIG. 2) having a trapezoidal shape and good mechanical strength can be obtained.

The partition wall having a trapezoidal cross-sectional shape can be suitably used as a partition wall for a back plate that is a member for a plasma display. The manufacturing method of the back plate is achieved by subjecting the substrate on which the partition walls are formed to a known process such as forming a fluorescent layer.
The back plate manufactured in this way is sealed with a front plate for plasma display manufactured by a known method, and discharge gas is sealed in a space formed between the front plate and the back plate. A plasma display panel can be obtained.

  EXAMPLES Hereinafter, although an Example demonstrates this invention in detail, this invention is not limited by these Examples.

Moreover, the raw material used for photosensitive paste preparation in the following Example and comparative example is as follows, and in each example, a raw material is represented by an abbreviation.
(A-1) Spherical silica (manufactured by Admatechs; SO-C6)
(A-2) Low melting point lead-free glass particles (manufactured by Yamato Electronics Co., Ltd., YEB2-6701)
(B-1) Ethylene glycol diacetate 50 wt% solution of phenol novolac resin (manufactured by Gunei Chemical Industry Co., Ltd., PSM-4326)
(B-2) 50% by weight solution of polyacrylic acid (manufactured by Aldrich Mw: 1250) in 50% by weight gamma-butyrolactone (C-1) 1,3-di (3′-glycidyloxypropyl) -1,1,3,3 -Tetramethyl-disiloxane (Rodel, SILCOLEASE PC-606PEX)
(D-1) Rhodosil Photoinitiator (Rodel, PI-2074)
(G-1) Sensitizer (manufactured by Kawasaki Chemical Industry Co., Ltd., DBA)
(E-1) Ethylene glycol diacetate (manufactured by Tokyo Chemical Industry)
(E-2) 1,2-propanediol dibenzoate (manufactured by Aldrich)
(E-3) gamma-butyrolactone (F-1) water (H-1) titanium oxide particles (manufactured by Ishihara Sangyo Co., Ltd., CR-EL)

Comparative Example 1
(A-1) 27.35 parts by mass (A-2) 41.03 parts by mass (B-1) 20.51 parts by mass (B-2) 1.71 parts by mass (C-1) 3.85 parts by mass (D-1) 0.85 parts by mass (G-1) 0.21 parts by mass (E-1) 2.14 parts by mass (E-2) 2.14 parts by mass (H-1) 0.21 parts by mass Was put in a polypropylene sealed container and stirred using a stirring defoaming machine (manufactured by Keyence Corporation; HM-500) to prepare a uniform photosensitive paste.
The composition weight ratio of the obtained photosensitive paste was (A) 68.38%, (B) 11.11%, (C) 3.85%, (D) 0.85%, (E) 15.38% (F) Water was 0% in the feed composition.
The prepared photosensitive paste was applied once on a dielectric-coated glass substrate using a 200 μm gap applicator. After coating, the coating film was prepared by drying in an oven at 90 ° C. for 40 minutes.

Next, the dried coating film was exposed with a proximity exposure machine (Dainippon Screen Mfg. Co., Ltd .; MAP-1300) using a 45 μm line, 240 μm pitch mask. The irradiation exposure dose was 400 mJ / cm ² . After exposure, the film was baked at 140 ° C. for 10 minutes and then developed with a 0.4 mass% aqueous sodium hydroxide solution. When the cross section of the pattern was observed with a scanning electron microscope (S-4500; manufactured by Hitachi, Ltd.), a pattern with a film thickness of 96 μm was obtained, but a thin cross section was observed. When the partition having a thin cross-sectional shape thus obtained is baked at 580 ° C. to obtain a partition wall, the partition wall has low mechanical strength.

Example 1
(A-1) 27.35 parts by mass (A-2) 41.03 parts by mass (B-1) 20.51 parts by mass (B-2) 1.71 parts by mass (C-1) 3.85 parts by mass (D-1) 0.85 parts by mass (G-1) 0.21 parts by mass (E-1) 2.14 parts by mass (E-2) 2.14 parts by mass (F-1) 0.43 parts by mass (H-1) 0.21 part by mass was placed in a polypropylene sealed container and stirred using a stirring defoamer (manufactured by Keyence Corporation; HM-500) to prepare a uniform photosensitive paste.
The composition weight ratio of the obtained photosensitive paste was (A) 68.09%, (B) 11.06%, (C) 3.83%, (D) 0.85%, (E) 15.32%. (F) 0.43%.
The prepared photosensitive paste was applied once on a dielectric-coated glass substrate using a 200 μm gap applicator. After coating, the coating film was prepared by drying in an oven at 90 ° C. for 40 minutes.

Next, the dried coating film was exposed with a proximity exposure machine (Dainippon Screen Mfg. Co., Ltd .; MAP-1300) using a 45 μm line, 240 μm pitch mask. The irradiation exposure dose was 400 mJ / cm ² . After exposure, the film was baked at 140 ° C. for 10 minutes and then developed with a 0.4 mass% aqueous sodium hydroxide solution. When the cross section of the pattern was observed with a scanning electron microscope (S-4500; manufactured by Hitachi, Ltd.), it was a pattern with a film thickness of 99 μm, and the cross sectional shape was a good trapezoidal shape. When the thus obtained pattern having a good cross-sectional shape is fired at 580 ° C. to obtain a partition wall, a high mechanical strength partition wall can be obtained.

Example 2
(A-1) 27.35 parts by mass (A-2) 41.03 parts by mass (B-1) 20.51 parts by mass (B-2) 1.71 parts by mass (C-1) 3.85 parts by mass (D-1) 0.85 parts by mass (G-1) 0.21 parts by mass (E-1) 2.14 parts by mass (E-2) 2.14 parts by mass (F-1) 0.85 parts by mass (H-1) 0.21 part by mass was placed in a polypropylene sealed container and stirred using a stirring defoamer (manufactured by Keyence Corporation; HM-500) to prepare a uniform photosensitive paste.
The composition weight ratio of the obtained photosensitive paste was (A) 67.80%, (B) 11.02%, (C) 3.81%, (D) 0.85%, (E) 15.25% (F) 0.85%.
The prepared photosensitive paste was applied once on a dielectric-coated glass substrate using a 200 μm gap applicator. After coating, the coating film was prepared by drying in an oven at 90 ° C. for 40 minutes.

Next, the dried coating film was exposed with a proximity exposure machine (Dainippon Screen Mfg. Co., Ltd .; MAP-1300) using a 45 μm line, 240 μm pitch mask. The irradiation exposure dose was 400 mJ / cm ² . After exposure, the film was baked at 140 ° C. for 10 minutes and then developed with a 0.4 mass% aqueous sodium hydroxide solution. When the cross section of the pattern was observed with a scanning electron microscope (S-4500; manufactured by Hitachi, Ltd.), it was a pattern with a film thickness of 99 μm, and the cross sectional shape was a good trapezoidal shape. When the thus obtained pattern having a good cross-sectional shape is fired at 580 ° C. to obtain a partition wall, a high mechanical strength partition wall can be obtained.

Example 3
(A-1) 27.35 parts by mass (A-2) 41.03 parts by mass (B-1) 20.51 parts by mass (B-2) 1.71 parts by mass (C-1) 3.85 parts by mass (D-1) 0.85 parts by mass (G-1) 0.21 parts by mass (E-1) 2.14 parts by mass (E-2) 2.14 parts by mass (F-1) 1.28 parts by mass (H-1) 0.21 part by mass was placed in a polypropylene sealed container and stirred using a stirring defoamer (manufactured by Keyence Corporation; HM-500) to prepare a uniform photosensitive paste.
The composition weight ratio of the obtained photosensitive paste was (A) 67.51%, (B) 10.97%, (C) 3.80%, (D) 0.84%, (E) 15.19%. (F) 1.27%.
The prepared photosensitive paste was applied once on a dielectric-coated glass substrate using a 200 μm gap applicator. After coating, the coating film was prepared by drying in an oven at 90 ° C. for 40 minutes.

Next, the dried coating film was exposed with a proximity exposure machine (Dainippon Screen Mfg. Co., Ltd .; MAP-1300) using a 45 μm line, 240 μm pitch mask. The irradiation exposure dose was 400 mJ / cm ² . After exposure, the film was baked at 140 ° C. for 10 minutes and then developed with a 0.4 mass% aqueous sodium hydroxide solution. When the cross section of the pattern was observed with a scanning electron microscope (S-4500; manufactured by Hitachi, Ltd.), the pattern had a thickness of 102 μm and the cross-sectional shape was a good trapezoidal shape. When the thus obtained pattern having a good cross-sectional shape is fired at 580 ° C. to obtain a partition wall, a high mechanical strength partition wall can be obtained.

Example 4
(A-1) 27.35 parts by mass (A-2) 41.03 parts by mass (B-1) 20.51 parts by mass (B-2) 1.71 parts by mass (C-1) 3.85 parts by mass (D-1) 0.85 parts by mass (G-1) 0.21 parts by mass (E-1) 2.14 parts by mass (E-2) 2.14 parts by mass (F-1) 1.71 parts by mass (H-1) 0.21 part by mass was placed in a polypropylene sealed container and stirred using a stirring defoamer (manufactured by Keyence Corporation; HM-500) to prepare a uniform photosensitive paste.
The composition weight ratio of the obtained photosensitive paste was (A) 67.23%, (B) 10.92%, (C) 3.78%, (D) 0.84%, (E) 15.13%. (F) 1.68%.
The prepared photosensitive paste was applied once on a dielectric-coated glass substrate using a 200 μm gap applicator. After coating, the coating film was prepared by drying in an oven at 90 ° C. for 40 minutes.

Next, the dried coating film was exposed with a proximity exposure machine (Dainippon Screen Mfg. Co., Ltd .; MAP-1300) using a 45 μm line, 240 μm pitch mask. The irradiation exposure dose was 400 mJ / cm ² . After exposure, the film was baked at 140 ° C. for 10 minutes and then developed with a 0.4 mass% aqueous sodium hydroxide solution. When the cross section of the pattern was observed with a scanning electron microscope (S-4500; manufactured by Hitachi, Ltd.), the pattern had a thickness of 104 μm and the cross-sectional shape was a good trapezoidal shape. When the thus obtained pattern having a good cross-sectional shape is fired at 580 ° C. to obtain a partition wall, a high mechanical strength partition wall can be obtained.

Example 5
(A-1) 27.35 parts by mass (A-2) 41.03 parts by mass (B-1) 20.51 parts by mass (B-2) 1.71 parts by mass (C-1) 3.85 parts by mass (D-1) 0.85 parts by mass (G-1) 0.21 parts by mass (E-1) 2.14 parts by mass (E-2) 2.14 parts by mass (F-1) 2.14 parts by mass (H-1) 0.21 part by mass was placed in a polypropylene sealed container and stirred using a stirring defoamer (manufactured by Keyence Corporation; HM-500) to prepare a uniform photosensitive paste.
The composition weight ratio of the obtained photosensitive paste is (A) 66.95%, (B) 10.88%, (C) 3.77%, (D) 0.84%, (E) 15.06%. (F) 2.09%.
The prepared photosensitive paste was applied once on a dielectric-coated glass substrate using a 200 μm gap applicator. After coating, the coating film was prepared by drying in an oven at 90 ° C. for 40 minutes.

Next, the dried coating film was exposed with a proximity exposure machine (Dainippon Screen Mfg. Co., Ltd .; MAP-1300) using a 45 μm line, 240 μm pitch mask. The irradiation exposure dose was 400 mJ / cm ² . After exposure, the film was baked at 140 ° C. for 10 minutes and then developed with a 0.4 mass% aqueous sodium hydroxide solution. When the cross section of the pattern was observed with a scanning electron microscope (S-4500; manufactured by Hitachi, Ltd.), it was a pattern with a film thickness of 103 μm, and the cross-sectional shape was a good trapezoidal shape. When the thus obtained pattern having a good cross-sectional shape is fired at 580 ° C. to obtain a partition wall, a high mechanical strength partition wall can be obtained.

It is a figure which shows typically the pattern of the shape in which cross-sectional shape has thinness. It is a figure which shows typically the pattern whose cross-sectional shape is trapezoid shape.

Explanation of symbols

DESCRIPTION OF SYMBOLS 1 ... Board | substrate, 2 ... Pattern (partition) in which cross-sectional shape has medium thinness, 3 ... Medium thin part, 4 ... Pattern in which cross-sectional shape is trapezoid shape (partition)

Claims (9)

(A) Inorganic particles (B) Alkali-soluble resin (C) Crosslinker (D) Acid generator (E) An organic solvent is included, and (F) 0.05 to 5% by mass of water with respect to the total amount of the photosensitive paste The photosensitive paste characterized by containing in the range.   The content ratios of (A) to (E) with respect to the photosensitive paste are (A) 20 to 95% by mass, (B) 2 to 30% by mass, (C) 1 to 30% by mass, (D 2. The photosensitive paste according to claim 1, which is 0.01 to 20% by mass and (E) 1 to 40% by mass. The (B) is a resin in which a novolak resin and / or a partial hydroxyl group of the novolak resin is substituted with an OR ₃ group (where R ₃ is a monovalent organic group having 1 to 20 carbon atoms), The photosensitive paste according to claim 1 or 2, wherein (C) is an epoxy-containing silicon compound represented by formula (3).

(In the formula, Q ₂ and Q ₃ are each independently a group represented by the formula (4), and Q ₁ is selected from the group represented by the formula (5)).

(In the formula, T ₁ represents an alkylene group having 1 to 6 carbon atoms, an alkyleneoxyalkylene group having 1 to 6 carbon atoms, or a phenylene group. M is 0 or 1.)

(Wherein T _{2 to} T ₇ represent a methyl group or a phenyl group. T ₈ is selected from a group consisting of an oxygen atom, a methylene group, an ethenylene group, an ethynylene group, a phenylene group, a naphthalenediyl group, and a biphenyldiyl group. .)   The photosensitive paste of Claims 1-3 whose said (E) is an organic solvent whose refractive index in 25 degreeC is 1.40-1.80.   The photosensitive paste in any one of Claims 1-4 whose said (A) is an inorganic particle containing the low melting glass particle whose softening point is 400 to 600 degreeC.   The partition for plasma display panels manufactured using the photosensitive paste in any one of Claims 1-5.   The member for plasma displays provided with the partition for plasma display panels of Claim 6.   A plasma display panel comprising the member for plasma display according to claim 7. The manufacturing method of the partition for plasma display panels provided with the following process (a) The process of apply | coating the photosensitive paste in any one of Claims 1-5 on a board | substrate, and forming a coating film (b) Application after application | coating Step of heating the film (c) Step of exposing the coating film obtained in the above (b) (d) Step of heating the coating film after exposure (e) Step of developing the coating film (f) After development, The step of firing the substrate at a temperature of 450 ° C. to 600 ° C.

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