KR20060049421A - Inorganic particle-containing compositions and process for preparing components for plasma display panel - Google Patents

Abstract

The present invention has a high aspect ratio, excellent shape uniformity, and can be completely decomposed and removed from a binder resin by a calcination process performed under relatively low temperature conditions (600 ° C. or lower), and does not contain an organic substance derived therefrom. It is to provide an inorganic powder-containing composition capable of forming a member and a method for forming a member for PDP.

Moreover, this invention contains (A) inorganic powder, (B) acrylic resin, (C) polyfunctional (meth) acrylate, and (D) photoinitiator, inorganic powder containing composition, transfer film obtained from it, and A method of forming a member for PDP is provided.

Plasma Display Panel Member, Inorganic Powder, Transfer Film

Description

Inorganic Particle-Containing Compositions and Process for Preparing Components for Plasma Display Panel}

1 is a schematic diagram showing a cross-sectional shape of an AC plasma display panel.

<Description of Major Symbols in Drawing>

1, 2: glass substrate 3: partition wall

4: transparent electrode 5: bus electrode

6: address electrode 7: fluorescent material

8, 9: dielectric 10: protective layer

[Patent Document 1] Japanese Unexamined Patent Publication No. 2003-86089

[Patent Document 2] Japanese Patent Application Laid-Open No. 2004-51444

The present invention relates to an inorganic powder-containing composition and a method for forming a member for a plasma display panel using the same. More specifically, the present invention relates to an inorganic powder-containing composition which can be preferably used for forming partition walls of plasma display panels and the like, and a forming method using the same.

In recent years, a plasma display has attracted attention as a flat fluorescent display. 1 is a schematic diagram showing a cross-sectional shape of an AC plasma display panel (hereinafter also referred to as "PDP"). In FIG. 1, (1) and (2) are the glass substrates arrange | positioned opposingly, (3) is a partition, and the cell is partitioned by the glass substrate 1, the glass substrate 2, and the partition 3. . 4 is a transparent electrode fixed to the glass substrate 1, 5 is a bus electrode formed on the transparent electrode 4 for the purpose of lowering the resistance of the transparent electrode 4, 6 is a glass substrate 2 (7) is a fluorescent material held in the cell, (8) a dielectric layer formed on the surface of the glass substrate (1) to cover the transparent electrode (4) and the bus electrode (5), (9) Is a dielectric layer formed on the surface of the glass substrate 2 so as to cover the address electrode 6, and 10 is a protective film containing, for example, magnesium oxide. In addition, in a color PDP, in order to obtain an image with high contrast, a color filter (red, green, blue), a black matrix, or the like may be provided between the glass substrate and the dielectric layer.

As a method of forming each member in these PDPs, the following methods are currently mainstream.

(1) A paste-like composition containing an inorganic powder, a binder resin, and a solvent is produced, and the pattern of the member forming material is formed by repeating the application of the composition on a substrate by screen printing and drying a plurality of times, followed by A method of sintering an inorganic powder by removing an organic substance by firing a pattern (screen printing method).

(2) After forming a member-forming material film containing an inorganic powder and a binder resin on a substrate to form a resist pattern thereon, the portion not covered with the resist by a blasting apparatus is sand blasted, and then the remaining resist The method of forming a member formation material pattern by peeling a layer, and then baking this pattern removes an organic substance and sinters an inorganic powder (sandblasting method).

(3) A photosensitive member formation material film containing an inorganic powder and a photosensitive resin is formed on a substrate, and the obtained film is exposed and developed to form a member formation material pattern, and then the organic material is removed by firing this pattern to remove the inorganic powder. A method of sintering (photolithography method).

(4) A member-forming material film containing an inorganic powder and a binder resin is formed on a substrate, and the pattern is formed by pressing the film into a mold having a pattern structure to be formed from above, followed by firing the pattern to remove the organic material. To sinter the inorganic powder (press molding method).

For example, when forming the partition wall, the thickness of the member formation material layer (the partition wall formation material layer) is 1.3 to 2.0 times the height of the partition wall to be formed in consideration of the amount of reduction in the film thickness due to the removal of the organic material in the firing step. In order to make the height of a partition 100 to 150 micrometers, it is necessary to form the partition formation material layer about 130-300 micrometers thick, for example.

In the case of forming the partition wall by the screen printing method, since the thickness of the coating film formed by one coating process is about 15 to 25 µm, in order to make the partition wall forming material layer a predetermined thickness, paste is applied to the surface of the glass substrate. Since it is necessary to apply | coat repeatedly (multiprinting) multiple times (for example, 10-20 times) the composition of a phase, it becomes difficult to equalize a partition height. In addition, the process is extended.

In the sand blasting method, problems such as lengthening of the process by exposure, developing, blasting, and the like and generation of waste due to blasting are problems.

Also in the photolithography method, exposure and development processes are required, and generation of waste is a problem.

In addition, in the press molding method, the process seems simple at first glance, but high precision management of the mold is required, and reliability is still insufficient, such as the shape of the barrier rib material layer greatly affecting the flatness of the substrate.

As a means for solving the above problems in the case of forming the partition by the conventional method, a method of forming the partition by UV curing while continuously extruding the photosensitive paste composition on the substrate by a special discharge nozzle (hereinafter, The "nozzle discharge method" is also proposed (patent documents 1 and 2).

According to such a nozzle discharge method, a partition having a high aspect ratio can be formed in a very simple process that cannot be compared with a conventional method.

However, if the conventionally known photosensitive paste composition is to be applied to the nozzle ejection method, many problems arise such as peeling of the pattern formed during firing or generation of voids inside the member after firing. It was difficult to stably form a member having excellent shape uniformity at an aspect ratio.

This invention is made | formed based on the above circumstances.

A first object of the present invention is to provide an inorganic powder-containing composition capable of forming a high aspect ratio PDP member and a method for forming a PDP member.

The 2nd object of this invention is to provide the inorganic powder containing composition which can form the member for PDP excellent in shape uniformity, and the formation method of the member for PDP.

A third object of the present invention is to completely decompose and remove the binder resin by firing treatment performed under relatively low temperature conditions (600 ° C. or lower), and to form a member for PDP that does not contain an organic substance derived therefrom. There is provided an inorganic powder-containing composition and a method for forming a member for PDP.

Other objects and effects of the present invention will become apparent from the following description.

The inorganic powder-containing composition of the present invention comprises (A) an inorganic powder, (B) a polymer having a structural unit represented by the following general formula (1) (hereinafter also referred to as "polymer (B)"), (C) polyfunctional (meth) It is characterized by containing an acrylate and (D) photoinitiator.

In the formula, R ¹ is a hydrogen atom or a methyl group, and R ² is a monovalent organic group.

The method for forming a member for a PDP of the present invention comprises the steps of relatively moving the nozzle and the substrate to form a pattern while discharging the inorganic powder-containing composition of the present invention from the nozzle onto the substrate, a step of irradiating the pattern with radiation, and It characterized by including a step of firing the pattern.

According to the composition of the present invention, the following effects are exerted.

(1) By controlling the viscosity of the composition in a specific range, a glass sintered compact (for example, a partition of PDP) having a high aspect ratio and excellent shape uniformity can be formed.

(2) By using the composition, the binder resin can be completely decomposed and removed by a calcination process performed under relatively low temperature conditions (600 ° C. or lower), and a glass sintered body containing no organic substance derived therefrom can be formed. .

(3) By using the composition, a glass sintered body suitable as a partition wall of PDP can be formed.

(4) By applying the composition to the nozzle discharge method, a glass sintered body (for example, PDP partition wall) can be formed by a very simple process not conventionally obtained.

EMBODIMENT OF THE INVENTION Hereinafter, this invention is demonstrated in detail.

Inorganic powder-containing composition

The inorganic powder-containing composition of the present invention is a paste-like composition comprising an inorganic powder, a polymer (B), a polyfunctional (meth) acrylate, and a photopolymerization initiator.

Hereinafter, each component of a composition is demonstrated.

<Inorganic powder>

The inorganic powder used for the inorganic powder-containing composition of the present invention differs depending on the type of forming member.

For example, as an inorganic powder used for a partition formation material and a dielectric layer formation material, glass powder, Preferably the glass powder whose softening point is 400-600 degreeC is mentioned. In the case where the softening point of the glass powder is less than 40 ° C., the glass powder melts in a step in which the organic material is not completely decomposed and removed in the firing step of the member forming material layer by the composition. Some may remain. As a result, when the member is a partition wall, the outgas diffuses into the panel, resulting in a reduction in the lifetime of the phosphor, or in the case of the dielectric layer, the dielectric characteristics or the display characteristics may be degraded. On the other hand, when the softening point of glass powder exceeds 600 degreeC, since baking needs to be carried out at high temperature rather than 600 degreeC, distortion etc. are easy to generate | occur | produce in a glass substrate.

Specific examples of preferred glass powders include: 1. lead oxide, boron oxide, silicon oxide, calcium oxide (PbO-B ₂ O ₃ -SiO ₂ -CaO-based), 2. zinc oxide, boron oxide, silicon oxide (ZnO-B ₂ O ₃ -SiO ₂ based), 3. Lead oxide, boron oxide, silicon oxide, aluminum oxide (PbO-B ₂ O ₃ -SiO ₂ -Al ₂ O ₃ based), 4. lead oxide, zinc oxide, boron oxide, Silicon oxide (PbO-ZnO-B ₂ O ₃ -SiO ₂ ), 5. lead oxide, zinc oxide, boron oxide, silicon oxide, titanium oxide (PbO-ZnO-B ₂ O ₃ -SiO ₂ -TiO _{2 type} ), etc. Can be illustrated. Moreover, inorganic oxide compound powders, such as aluminum oxide, chromium oxide, and manganese oxide, can also be mixed and used for these glass powders, for example.

Examples of the inorganic powder used for the electrode forming material include Ag, Au, Al, Ni, Ag-Pd alloys, Cu, Cr, and the like.

Examples of the inorganic powder used in the resistor forming material include Ru0 ₂ and the like.

Examples of the inorganic powder used in the phosphor-forming material include Y ₂ O ₃ : Eu ³⁺ , Y ₂ SiO ₅ : Eu ³⁺ , Y ₃ Al ₅ O ₁₂ : Eu ³⁺ , YVO ₄ : Eu ³⁺ , (Y, Gd Red phosphors such as) BO ₃ : Eu ³⁺ and Zn ₃ (P0 ₄ ) ₂ : Mn; Green phosphors such as Zn ₂ SiO ₄ : Mn, BaAl ₁₂ O ₁₉ : Mn, BaMgAl ₁₄ O ₂₃ : Mn, LaPO ₄ : (Ce, Tb), Y ₃ (Al, Ga) ₅ O ₁₂ : Tb; Y ₂ SiO ₅ : Ce, BaMgAl ₁₀ O ₁₇ : Eu ²⁺ , BaMgAl ₁₄ O ₂₃ : Eu ²⁺ , (Ca, Sr, Ba) ₁₀ (PO ₄ ) ₆ Cl ₂ : Eu ²⁺ , (Zn, Cd) Blue phosphors, such as S: Ag, are mentioned.

Examples of the inorganic powder to form a color filter used in the materials _{Fe 2 O 3, Pb 3 O} 4, CdS, CdSe, PbCrO 4, PbSO 4, Fe (NO 3) for a red pigment such as _3; Green pigments such as Cr ₂ O ₃ , TiO ₂ -CoO-NiO-ZnO, CoO-CrO-TiO ₂ -Al ₂ O ₃ , Co ₃ (PO ₄ ) ₂ , CoO-ZnO; PbCrO ₄ -PbSO ₄ , PbCrO ₄ , PbCrO ₄ -PbO, CdS as inorganic pigments for color correction, in addition to blue pigments such as 2 (Al ₂ Na ₂ Si ₃ O ₁₀ ), Na ₂ S ₄ and CoO-Al ₂ O ₃ Yellow pigments such as TiO ₂ -NiO-Sb ₂ O ₃ ; Orange pigments such as Pb (Cr-Mo-S) O ₄ ; And purple pigments such as Co ₃ (PO ₄ ) ₂ .

Mn, Fe, Cr, etc. are mentioned as an inorganic powder used for a black matrix forming material.

In addition, member formation materials other than a partition formation material and a dielectric layer formation material may contain glass powder with the inorganic powder mentioned above. The content rate of glass powder is 20 weight% or less with respect to inorganic powder whole quantity, Preferably it is 10 weight% or less.

<Polymer (B)>

Polymer (B) is an acrylic resin and is contained as binder resin of the composition of this invention. The member for PDP obtained by containing a polymer (B) has the outstanding adhesiveness and shape uniformity with respect to a board | substrate.

As such a polymer, it is possible to bind the inorganic powder with appropriate adhesiveness, and is selected from the (co) polymers which are completely oxidized and removed by the firing temperature (for example, 400 to 600 ° C.) of the composition, and is represented by Chemical Formula 1 Has units. The structural unit is obtained by using a compound represented by the following general formula (1a) (hereinafter also referred to as "compound (1a)") as a polymerization component, and as the polymer (B), a homopolymer of compound (1a), two or more compounds ( Copolymers of 1a) and copolymers of compound (1a) with other copolymerizable monomers.

In the formula, R ¹ is a hydrogen atom or a methyl group, and R ² is a monovalent organic group.

Specific examples of the (meth) acrylate compound represented by Chemical Formula 1a include methyl (meth) acrylate, ethyl (meth) acrylate, n-propyl (meth) acrylate, i-propyl (meth) acrylate, n-butyl (Meth) acrylate, i-butyl (meth) acrylate, t-butyl (meth) acrylate, n-pentyl (meth) acrylate, i-pentyl (meth) acrylate, n-hexyl (meth) acrylate , n-heptyl (meth) acrylate, n-octyl (meth) acrylate, i-octyl (meth) acrylate, 2-ethylhexyl (meth) acrylate, n-nonyl (meth) acrylate, n-decyl (Meth) acrylate, i-decyl (meth) acrylate, undecyl (meth) acrylate, dodecyl (meth) acrylate, lauryl (meth) acrylate, stearyl (meth) acrylate, i-ste Alkyl (meth) acrylates such as aryl (meth) acrylate;

Hydroxyethyl (meth) acrylate, 2-hydroxypropyl (meth) acrylate, 4-hydroxybutyl (meth) acrylate, 3-hydroxypropyl (meth) acrylate, 2-hydroxybutyl (meth) Hydroxyalkyl (meth) acrylates such as acrylate and 3-hydroxybutyl (meth) acrylate;

Phenoxyalkyl (meth) acrylates such as phenoxyethyl (meth) acrylate and 2-hydroxy-3-phenoxypropyl (meth) acrylate;

2-methoxyethyl (meth) acrylate, 2-ethoxyethyl (meth) acrylate, 2-propoxyethyl (meth) acrylate, 2-butoxyethyl (meth) acrylate, 2-methoxybutyl ( Alkoxyalkyl (meth) acrylates such as meth) acrylate;

Polyethylene glycol mono (meth) acrylate, ethoxy diethylene glycol (meth) acrylate, methoxy polyethylene glycol (meth) acrylate, phenoxy polyethylene glycol (meth) acrylate, nonylphenoxy polyethylene glycol (meth) acrylate, Polyalkylene glycols such as polypropylene glycol mono (meth) acrylate, methoxypolypropylene glycol (meth) acrylate, ethoxy polypropylene glycol (meth) acrylate, and nonylphenoxy polypropylene glycol (meth) acrylate ( Meth) acrylates;

Cyclohexyl (meth) acrylate, 4-butylcyclohexyl (meth) acrylate, dicyclopentanyl (meth) acrylate, dicyclopentenyl (meth) acrylate, dicyclopentadienyl (meth) acrylate, bor Cycloalkyl (meth) acrylates such as niel (meth) acrylate, isobornyl (meth) acrylate and tricyclodecanyl (meth) acrylate;

Benzyl (meth) acrylate, tetrahydrofurfuryl (meth) acrylate, etc. are mentioned.

Of these, the group represented by R ² in Formula 1a is preferably a group containing an alkyl group, an alkoxyalkyl group or a hydroxyalkyl group, and methyl (meth) acrylate and n-butyl (meth) are particularly preferred as (meth) acrylate compounds. Acrylate, 2-ethyl hexyl (meth) acrylate, lauryl (meth) acrylate, i-decyl (meth) acrylate and 2-ethoxyethyl (meth) acrylate.

The other copolymerizable monomer used for the copolymerization with the compound (1a) is not particularly limited as long as it is a compound copolymerizable with the compound (1a). Examples thereof include unsaturated carboxyl such as (meth) acrylic acid, vinylbenzoic acid, maleic acid, and vinylphthalic acid. Acid; And vinyl group-containing radically polymerizable compounds such as vinyl benzyl methyl ether, vinyl glycidyl ether, styrene, α-methyl styrene, butadiene and isoprene.

As for the polymer (B), the structural unit represented by the said Formula (1) is 70 weight% or more normally, Preferably it is 90 weight% or more, More preferably, it is 100 weight%.

As molecular weight of a polymer (B), it is preferable that it is 2,000-300,000 as a weight average molecular weight of polystyrene conversion by GPC, and it is more preferable that it is 5,000-200,00.

The polymer (B) preferably has a viscosity of 1,000 to 30,000 cP, measured at a rotational speed of 0.5 rpm (shearing speed of 2 sec ^-1 ) using a cone rotatable viscometer under conditions of 25 ° C and 1 atmosphere, and 5,000 to 20,000. It is especially preferable that it is cP. In addition, when using 2 or more types of polymers, it is preferable that the mixture viscosity of the polymer to be used exists in the said range.

5-40 weight part is preferable with respect to 100 weight part of inorganic powders, and, as for content of the polymer (B) in the composition of this invention, 7-20 weight part is especially preferable.

When content of a polymer (B) is less than 5 weight part, the dispersibility of an inorganic powder will fall, the intensity | strength of the pattern after irradiation may become insufficient, and adhesiveness with a board | substrate may become bad. In addition, when the content exceeds 40 parts by weight, the substrate is in close contact with the substrate, but there are many cavities due to the disappearance of the polymer in the formed member, so that the strength of the member is insufficient, or gas is released from the interior of the cavity in the long term, resulting in deterioration of the performance of the PDP. It may lead to.

<Multifunctional (meth) acrylate>

The polyfunctional (meth) acrylate used in the present invention has the effect of curing by irradiation with radiation, preventing deformation of the pattern shape up to and during firing, thereby forming a pattern having excellent shape uniformity at a high aspect ratio. will be.

As a specific example of the said polyfunctional (meth) acrylate, Di (meth) acrylates of alkylene glycol, such as ethylene glycol and propylene glycol; Di (meth) acrylates of polyalkylene glycols such as polyethylene glycol and polypropylene glycol; Di (meth) acrylates of both terminal hydroxylated polymers such as both terminal hydroxypolybutadiene, both terminal hydroxypolyisoprene and both terminal hydroxypolycaprolactone; Poly (meth) acrylates of trivalent or higher polyhydric alcohols such as glycerin, 1,2,4-butanetriol, trimethylolalkane, tetramethylolalkane, dipentaerythritol, etc .; Poly (meth) acrylates of polyalkylene glycol adducts of trivalent or higher polyhydric alcohols; Poly (meth) acrylates of cyclic polyols such as 1,4-cyclohexanediol and 1,4-benzenediols; Oligos, such as polyester (meth) acrylate, epoxy (meth) acrylate, urethane (meth) acrylate, alkyd resin (meth) acrylate, silicone resin (meth) acrylate, and spiran resin (meth) acrylate (Meth) acrylates etc. are mentioned, These can be used individually or in combination of 2 or more types.

The polyfunctional (meth) acrylate preferably has a viscosity of 100 to 5,000 cP measured at a rotational speed of 2.5 rpm (shearing speed of 10 sec ⁻¹ ) using a cone rotatable viscometer under conditions of 25 ° C. and 1 atmosphere. , 500 to 2,000 cP is particularly preferred. In addition, when using 2 or more types of polyfunctional (meth) acrylate, it is preferable that the mixture viscosity of the polyfunctional (meth) acrylate to be used exists in the said range.

The content rate of the said polyfunctional (meth) acrylate is 5-50 weight part normally with respect to 100 weight part of inorganic powder, Preferably it is 10-30 weight part. If it is less than 5 parts by weight, the photosensitivity is insufficient, so that it is difficult to maintain the pattern shape. If it exceeds 50 parts by weight, the viscosity characteristic of the composition is poor, which tends to adversely affect the ejectability from the nozzle.

<Photoinitiator>

Specific examples of the photopolymerization initiator used in the present invention include benzyl, benzoin, benzophenone, camphorquinone, 2-hydroxy-2-methyl-1-phenylpropan-1-one, 1-hydroxycyclohexylphenyl ketone, 2, 2-dimethoxy-2-phenylacetophenone, 2-methyl- [4 '-(methylthio) phenyl] -2-morpholino-1-propaneone, 2-benzyl-2-dimethylamino-1- (4 Carbonyl compounds such as -morpholinophenyl) -butan-1-one; Azo compounds or azide compounds such as azoisobutyronitrile and 4-azide benzaldehyde; Organic sulfur compounds such as mercaptan disulfide; Organic peroxides such as benzoyl peroxide, di-tert-butyl peroxide, tert-butyl hydroperoxide, cumene hydroperoxide and paramethane hydroperoxide; 1,3-bis (trichloromethyl) -5- (2'-chlorophenyl) -1,3,5-triazine, 2- [2- (2-furanyl) ethylenyl] -4,6-bis Trihalo methanes such as (trichloromethyl) -1,3,5-triazine; Imidazole dimers such as 2,2'-bis (2-chlorophenyl) -4,5,4 ', 5'-tetraphenyl-1,2'-biimidazole and the like. It can be used in combination of 2 or more type.

The content rate of the said photoinitiator is 5-30 weight part normally with respect to 100 weight part of polyfunctional (meth) acrylates, Preferably it is 10-20 weight part. If it is less than 5 parts by weight, the photosensitivity is insufficient and the development of a good pattern shape tends to be difficult. If it exceeds 30 parts by weight, the remaining photopolymerization initiator tends to adversely affect the firing.

The composition of the present invention contains, as an optional component, other binder resins, solvents, dispersants, tackifiers, surface tension regulators, stabilizers, plasticizers, adhesion aids, antihalation agents, storage stabilizers, antifoaming agents, antioxidants, ultraviolet absorbers, fillers, phosphors, Various additives such as pigments and dyes may be contained.

As the solvent optionally contained in the composition of the present invention, it is preferable that the affinity with the inorganic powder and the solubility of the binder resin are good, the viscosity can be imparted to the composition, and the evaporation can be easily removed by drying and baking. In particular, preferred solvents include ketones, alcohols, and esters (hereinafter, referred to as "specific solvents") having a standard boiling point (boiling point at 1 atmosphere) of 100 to 200 ° C.

As a specific example of such a specific solvent, Ketones, such as a diethyl ketone, a methyl butyl ketone, a dipropyl ketone, cyclohexanone; alcohols such as n-pentanol, 4-methyl-2-pentanol, cyclohexanol and diacetone alcohol; Ether alcohols such as ethylene glycol monomethyl ether, ethylene glycol monoethyl ether, ethylene glycol monobutyl ether, propylene glycol monomethyl ether and propylene glycol monoethyl ether; Saturated aliphatic monocarboxylic acid alkyl esters such as acetic acid-n-butyl and amyl acetate; Lactic acid esters such as ethyl lactate and lactic acid-n-butyl; Ether esters such as methyl cellosolve acetate, ethyl cellosolve acetate, propylene glycol monomethyl ether acetate, and ethyl-3-ethoxypropionate; and the like, and methylbutyl ketone and cyclohexanone can be exemplified. And diacetone alcohol, ethylene glycol monobutyl ether, propylene glycol monomethyl ether, ethyl lactate, ethyl-3-ethoxypropionate, and the like are preferable. These specific solvents can be used individually or in combination of 2 or more types.

Specific examples of solvents other than the specific solvents include terebin oil, ethyl cellosolve, methyl cellosolve, terpineol, butyl carbitol acetate, butyl carbitol, i-propyl alcohol, benzyl alcohol, and the like.

As a content rate of the solvent in the composition of this invention, it is preferable that it is 50 weight part or less with respect to 100 weight part of inorganic powder from a viewpoint of maintaining the viscosity of a composition in a preferable range, and it is more preferable that it is 10 weight part or less.

Moreover, it is preferable that it is 50 weight% or more, and, as for the content rate of the specific solvent with respect to all the solvents, it is more preferable that it is 70 weight% or more.

The composition of this invention can be manufactured by kneading the said glass powder, binder resin, a photoinitiator, and arbitrary components using kneading | dispersing machines, such as a roll kneader, a mixer, a homomixer, a sand mill, and an oil-type stirring disperser.

The composition of this invention manufactured as mentioned above is a paste-like composition which has the fluidity suitable for application | coating.

It is preferable that the viscosity at the time of using the inorganic powder containing composition of this invention for a nozzle discharge method is 100,000-3,000,000 cP. If the viscosity of the composition is less than 100,000 cP, there may be a possibility that liquid spillage, planarization, or the like occurs between the time when the paste is discharged by the nozzle and the exposure, thereby failing to form a high aspect ratio structure. Moreover, when paste viscosity exceeds 3,000,000 cP, handling property may fall, such as poor discharge property from a nozzle.

In addition, measurement of the viscosity in this invention is performed at cone | corn rotation speed 0.5rpm using rotor NO.7 using the cone rotary viscometer RE-80U by AX Sangyo Co., Ltd. on 25 degreeC and 1 atmosphere of conditions. More preferably, the measurement value when 1 minute passes after the start of rotation is defined as the viscosity of the composition. This is because the pasty composition often exhibits non-Newtonianity.

As described above, the composition of the present invention can be particularly preferably used when producing a member for PDP mainly by the nozzle ejection method or the like. However, the composition is not limited to these uses, and is preferably used for the formation of a conventionally known pattern or inorganic film. Can be.

Formation method of member for PDP

The method for forming the member for PDP of the present invention,

1. Process of forming a pattern by relatively moving a nozzle and a board | substrate, discharging the inorganic powder containing composition of this invention on a board | substrate,

2. irradiating the pattern with radiation, and

3. It characterized by including the step of firing the pattern.

As discharge conditions in the said process 1, discharge pressure is 0.1-1 Mpa and discharge speed is 0.2-20 mm / sec using the nozzle of the dimension substantially the same as the pattern shape to form, for example.

It does not specifically limit as a radiation irradiation apparatus used at the said process 2, For example, the exposure apparatus etc. used when manufacturing a semiconductor and a liquid crystal display device are used. Moreover, as radiation used for exposure, an ultraviolet-ray etc. are used preferably, for example.

Moreover, as baking process temperature in the said process 3, it is necessary to be temperature which the organic substance in a composition vanishes, and is 400-600 degreeC normally. Moreover, baking time is 10 to 60 minutes normally.

The partition which is preferably formed by the formation method of the present invention generally divides the horizontal direction of the display cell (display unit) of the panel. The magnitude | size of the lateral pitch of the display cell divided by the partition is 0.10 to 1.00 mm, for example.

Dimensions, such as the cross-sectional shape, width, height of a partition, and the separation distance of a partition, can be suitably selected according to the characteristic of the PDP made into the objective.

Specifically, the width of the bottom surface in the cross-sectional shape of the partition wall is 10 to 300 µm, the height is 10 to 500 µm, and the separation distance of the partition wall is 50 to 1000 µm, and the width of the electrode disposed between the partition walls is 50 to It becomes 500 micrometers. In a particularly typical example, the width of the bottom surface in the cross-sectional shape of the partition wall is 50 µm, the height is 150 µm, and the separation distance of the partition wall is 300 µm, and the width of the electrodes disposed between the partition walls is 100 µm. .

<Example>

Hereinafter, although the Example of this invention is described, this invention is not limited by these. In addition, "part" shows a "weight part" below.

In addition, the evaluation method in an Example is as follows.

[Dispersibility of Composition]

The particle size scale which 20 or more lines generate | occur | produce by the grinder gauge was measured, and it was judged that dispersibility was favorable when the measured value was less than 7.5.

[Bulk wall shape]

First, the cracks on the surface of the partition wall and the presence or absence of peeling from the substrate were first visually observed. Then, the width | variety and the height of the manufactured partition were calculated | required using the non-contact three-dimensional shape measuring apparatus "NH-3" (Ryo Co., Ltd. product). In addition, the partition fracture surface was observed using a scanning electron microscope. From the observation of the partition fracture surface, the presence or absence of a cavity inside the partition and its number and size were observed.

Emission Gas Analysis

A small amount of the gas discharged from the analysis of the barrier rib after firing was confirmed to detect the presence or absence of CO, CO ₂ by the analysis by the "flow-route switching method".

<Example 1>

(1) Preparation of Inorganic Powder-Containing Composition:

As a glass powder, _{PbO-B 2 O 3 -SiO 2} -Al 2 O 3 -TiO 2 based glass powder 100 (DTA softening transition ℃ 460, manufactured by Asahi Glass Co., Ltd.) average particle diameter of 1.0 ㎛ parts, the binder resin 20 parts of a polymer obtained by copolymerizing n-butyl methacrylate, lauryl methacrylate and hydroxypropyl methacrylate at a ratio of 50/30/20 by weight, and dipentaeryte as a polyfunctional (meth) acrylate. The composition of the present invention was prepared by kneading 20 parts of lithol hexaacrylate and 10 parts of 2-benzyl-2-dimethylamino-1- (4-morpholinophenyl) -butanone as a photopolymerization initiator using a dispersing machine.

When the dispersion degree was examined about the obtained composition, it was confirmed that it is 5 micrometers and it is a composition excellent in dispersibility.

(2) Formation of partition wall forming material layer:

Using the said composition, the partition wall forming material layer was produced on the glass substrate by the nozzle discharge method. That is, the composition was continuously discharged from a special nozzle, and irradiated with i-ray (ultraviolet light having a wavelength of 365 nm) with an ultra-high pressure mercury lamp to cure. Irradiation amount was 500 mJ / cm <^2> here.

(3) Firing treatment of partition wall forming material layer and evaluation of partition wall:

The glass substrate in which the partition formation material layer manufactured by said (2) was formed is arrange | positioned in a baking furnace, the temperature in a furnace is heated up to 560 degreeC with the temperature increase rate of 10 degree-C / min from normal temperature, and it is 10 minutes in 560 degreeC temperature atmosphere. By baking, the partition containing a glass sintered compact was formed in the glass substrate surface.

When the appearance of this partition was visually observed, no crack, peeling from the substrate, or the like was confirmed. In addition, CO and CO ₂ were not detected in the analysis of the released gas.

As a result of measuring the shape of the partition wall, it was found that the ideal structure had a high aspect ratio of 40 µm in width and 130 µm in height. Moreover, as a result of the cross-sectional observation by a scanning electron microscope, it was confirmed that it is a compact sintered compact.

<Examples 2 and 3 and Comparative Examples>

Inorganic powder-containing composition and comparative composition of the present invention in the same manner as in Example 1, except that the composition ratios of the glass powder, the binder resin, the polyfunctional (meth) acrylate and the photopolymerization initiator were changed according to the method shown in Table 1 below. Was prepared.

Next, the partition molding material layer was produced like Example 1 except having used each obtained composition.

Then, except having used each obtained partition formation material layer, it carried out similarly to Example 1, and baked the partition formation material layer, and manufactured the partition on the surface of the glass substrate for 20-inch panels.

About each composition concerning Example 2, 3, and a comparative example, the property of the formed partition was observed.

The above results are shown in Table 1.

The composition of the present invention is a PDP partition wall having a high aspect ratio, excellent shape uniformity, and capable of completely decomposing and removing a binder resin by a calcination process performed under relatively low temperature conditions, and containing no organic substance derived therefrom. Preferable glass sintered compact can be formed.

Claims (5)

An inorganic powder-containing composition comprising (A) an inorganic powder, (B) a polymer having a structural unit represented by the following formula (1), (C) a polyfunctional (meth) acrylate, and (D) a photopolymerization initiator. <Formula 1>

In the formula, R ¹ is a hydrogen atom or a methyl group, and R ² is a monovalent organic group. The inorganic powder-containing composition according to claim 1, wherein the content of the polymer (B) is 5 to 40 parts by weight based on 100 parts by weight of the (A) inorganic powder. The inorganic powder-containing composition according to claim 1, wherein (A) the inorganic powder is a glass frit. A process of forming a pattern by relatively moving a nozzle and a board | substrate, discharging the inorganic powder containing composition of Claim 1 from a nozzle on a board | substrate, Irradiating the pattern with radiation; A method for forming a member for a plasma display panel, comprising the step of firing the pattern. The method for forming a member for a plasma display panel according to claim 4, wherein the member obtained is a partition wall.

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