JPH10310450A - Glass paste composition - Google Patents

Abstract

PROBLEM TO BE SOLVED: To obtain a glass paste compsn. excellent in rapid dryability, not causing film defects in a film forming material layer formed by drying a coating film, capable of forming a dielectric layer having high light transmissivity and capable of producing a transfer film having satisfactory blocking resistance. SOLUTION: This glass paste compsn. contains glass powder, a bonding resin and at least one org. solvent selected from among ketones, alcohols and esters each having 100-200 deg.C standard b.p. and 0.5-50 mmHg vapor pressure at 20 deg.C and preferably having >=25 dyn/cm surface tension at 20 deg.C.

Description

DETAILED DESCRIPTION OF THE INVENTION

[0001]

The present invention relates to a glass paste composition, and more particularly, to a glass paste composition that can be suitably used for forming a dielectric layer of a plasma display panel.

[0002]

2. Description of the Related Art Recently, a plasma display has attracted attention as a flat fluorescent display. FIG. 1 is a schematic diagram showing a cross-sectional shape of an AC type plasma display panel (hereinafter, also referred to as “PDP”). In FIG. 1, reference numerals 1 and 2 denote glass substrates arranged opposite to each other, and reference numeral 3 denotes a partition. A cell is defined by the glass substrate 1, the glass substrate 2 and the partition 3. 4 is a bus electrode fixed to the glass substrate 1, 5 is an address electrode fixed to the glass substrate 2, 6 is a fluorescent substance held in a cell, and 7 is a surface of the glass substrate 1 so as to cover the bus electrode 4. The formed dielectric layer 8 is a protective film made of, for example, magnesium oxide. The dielectric layer 7 is formed of a glass sintered body and has a thickness of, for example, 20 to 50 μm.

As a method for forming the dielectric layer 7, a paste-like composition (glass paste composition) containing glass powder, a binder resin and a solvent is prepared, and the glass paste composition is glass-screened by a screen printing method. A method is known in which a film-forming material layer is formed by applying the film-forming material to the surface of a substrate 1 and drying, and then the film-forming material layer is baked to remove organic substances and sinter glass powder.

[0004] As a solvent constituting the glass paste composition, a relatively high boiling point (for example, 220) is used from the viewpoint of exhibiting a desirable viscosity (viscosity that does not cause clogging of the screen plate) of the glass paste composition for a long period of time.
(° C. or higher).
-31619). The drying conditions of the coating film for obtaining the film forming material layer are usually 100 to 150.
C. for 10-15 minutes.

Here, the thickness of the film forming material layer formed on the glass substrate 1 is determined in consideration of the reduction in the film thickness accompanying the removal of the organic substance in the firing step. It is necessary that the thickness is about 1.3 to 2.0 times the thickness. For example, in order to make the thickness of the dielectric layer 7 20 to 50 μm, a film forming material layer having a thickness of about 30 to 100 μm Need to be formed. On the other hand, when the glass paste composition is applied by a screen printing method, the thickness of a coating film formed by one application treatment is about 15 to 25 μm. Therefore, in order to make the film-forming material layer have a predetermined thickness, the glass paste composition needs to be repeatedly applied (multiple printing) a plurality of times (for example, 2 to 7 times) to the surface of the glass substrate. There is.

However, in the case of forming a film forming material layer by multiple printing using a screen printing method,
The dielectric layer formed by firing the film forming material layer does not have a uniform thickness (for example, the tolerance is within ± 5%). This is due to the multiple printing by the screen printing method,
This is because it is difficult to uniformly apply the glass paste composition to the surface of the glass substrate, and the larger the application area (panel size) and the greater the number of applications, the greater the degree of variation in the thickness of the dielectric layer. Will be large. Then, in the panel material (glass substrate having the dielectric layer) obtained through the application process by the multiple printing, the dielectric characteristics due to the film thickness variations occur in the plane, and the dielectric characteristics vary. This causes display defects (luminance unevenness) in the PDP. Further, in the screen printing method, the mesh shape of the screen plate may be transferred to the surface of the film forming material layer, and the dielectric layer formed by firing such a film forming material layer has a smooth surface. Inferior to

As a means for solving the above-mentioned problems in the case where the film-forming material layer is formed by the screen printing method, the present inventors apply a glass paste composition on a supporting film, dry the coating film, and dry the coating film. Forming a film forming material layer on the support film, transferring the film forming material layer formed on the support film to the surface of the glass substrate to which the electrodes are fixed, and baking the transferred film forming material layer to form the glass forming material layer. A method of manufacturing a PDP including a step of forming a dielectric layer on the surface of a substrate (hereinafter, also referred to as “dry film method”) has been proposed (see Japanese Patent Application No. 8-196304). According to such a manufacturing method, a dielectric layer having excellent film thickness uniformity and surface uniformity can be formed, and a composite film (a film-forming material layer formed on a supporting film) can be formed. Hereinafter, also referred to as a “transfer film”) is advantageous in that it can be wound and stored in a roll shape. Here, the drying conditions of the coating film (glass paste composition) applied on the support film are set at 110 ° C. or less from the viewpoint of heat resistance and production efficiency of the support film.
Be constrained within minutes.

[0008]

However, under the above-mentioned low-temperature and short-time drying conditions, an organic solvent having a boiling point of usually 220 ° C. or more cannot be sufficiently removed, and the organic solvent formed on the supporting film cannot be removed. A considerable amount (eg, 5 to 15% by weight) of the organic solvent remains in the film forming material layer. When a transfer film including such a film-forming material layer is wound into a roll and stored, the transfer films (the film-forming material layer and the back surface of the support) are fixed to each other. This causes a new problem that the transfer film cannot be pulled out from the roll.

In order to avoid such a problem, the residual amount of the solvent in the film forming material layer is reduced as much as possible by preparing the glass paste composition using a low boiling organic solvent. Is also conceivable. However, organic solvents having a low boiling point generally have poor affinity for glass powder, and glass paste containing such an organic solvent is liable to produce aggregates of glass powder. And a film-forming material layer formed by applying a glass paste composition containing an aggregate of glass powder on a support film, a streaky coating trace due to the aggregate, a crater,
Film defects such as pinholes occur. In addition, a glass paste containing a low-boiling organic solvent is applied to form a film-forming material layer, and the glass-sintered body (dielectric layer) formed by firing this film-forming material layer contains fine bubbles. , The dielectric layer is liable to be clouded, and the dielectric layer does not have sufficient transparency (light transmittance).

The present invention has been made in view of the above circumstances, and a first object of the present invention is to provide low-temperature, short-time drying conditions (for example, 50 to 110 ° C. for 1 to 10 minutes).
To provide a glass paste composition excellent in quick drying, which can remove most of the contained solvent (for example, the content of the solvent after drying becomes 0 to 1% by weight). is there. A second object of the present invention is to provide a glass paste composition that does not contain aggregates of glass powder. A third object of the present invention is to provide a glass paste composition that does not cause film defects such as streak-like coating marks, craters and pinholes in a film-forming material layer formed by drying a coating film. is there. A fourth object of the present invention is to provide a glass paste composition capable of forming a dielectric layer having high light transmittance (sufficient transparency) by firing the obtained film-forming material layer. It is in. A fifth object of the present invention is to provide a glass paste composition which can be suitably used for the production of a transfer film and which does not cause a blocking phenomenon when the obtained transfer film is wound up in a roll and stored. It is in.

[0011]

The glass paste composition of the present invention comprises (A) a glass powder, (B) a binder resin, and (C) a ketone which satisfies the following conditions (1) and (2). , At least one organic solvent selected from alcohols and esters (hereinafter also referred to as “specific solvent”)
It is characterized by containing. Further, the specific solvent,
It is preferable to satisfy the following condition (3). Condition (1): The standard boiling point is 100 to 200 ° C. Condition (2): vapor pressure at 20 ° C. is 0.5 to 50 mm
Hg. Condition (3): The surface tension at 20 ° C. is 25 dyn / c.
m or more.

[0012]

BEST MODE FOR CARRYING OUT THE INVENTION Hereinafter, a glass paste set of the present invention will be described.
The product will be described in detail. Glass paste of the present invention
The composition contains glass powder, binder resin and solvent as essential components
Contained as <Glass powder> a glass powder constituting the composition of the present invention;
The softening point is in the range of 400-600 ° C
Are preferred. When the softening point of the glass powder is less than 400 ° C
In some cases, baking of the film forming material layer with the composition
Process, organic substances such as binder resin are completely decomposed and removed
Glass powder melts at a stage where it is not
Some of the organic material remains in the dielectric layer
As a result, the light transmittance of the dielectric layer tends to decrease. on the other hand,
When the softening point of the glass powder exceeds 600 ° C, 60
Because it is necessary to fire at a temperature higher than 0 ° C, a glass substrate
Is easily distorted. Specific examples of suitable glass powder
As lead oxide, boron oxide, silicon oxide (Pb
OB_TwoO_Three-SiO_TwoSystem), zinc oxide,
Boron oxide, silicon oxide (ZnO-B_TwoO_Three-SiO_Two
Mixture), lead oxide, boron oxide, silicon oxide,
Aluminum oxide (PbO-B_TwoO_Three-SiO_Two-Al
_TwoO_ThreeSystem), lead oxide, zinc oxide, borate oxide
Element, silicon oxide (PbO-ZnO-B _TwoO_Three-SiO_Two
System) and the like.

<Binder Resin> In the composition of the present invention, the binder resin is preferably an acrylic resin. By containing an acrylic resin as a binder resin, the formed film-forming material layer becomes excellent in flexibility, and when forming the transfer film by forming the film-forming material layer on a support film. In addition, the roll processability of the transfer film is significantly improved. Further, the film-forming material layer containing the acrylic resin has excellent adhesiveness or adhesion to a glass substrate.

[0014] Such an acrylic resin is capable of binding glass powder with appropriate tackiness, and is completely oxidized and removed by baking (400 ° C to 600 ° C) the film forming material (co). It is selected from polymers. Such acrylic resins include a homopolymer of a (meth) acrylate compound represented by the following general formula (I), a copolymer of two or more (meth) acrylate compounds represented by the following general formula (I), And a copolymer of a (meth) acrylate compound represented by the following general formula (I) and a copolymerizable monomer.

[0015]

Embedded image

[Wherein, R ¹ represents a hydrogen atom or a methyl group, and R ² represents a monovalent organic compound. ]

Specific examples of the (meth) acrylate compound represented by the general formula (I) include methyl (meth) acrylate, ethyl (meth) acrylate, propyl (meth) acrylate, isopropyl (meth) acrylate, and butyl (meth) acrylate. (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, ethylhexyl (meth) acrylate, nonyl (meth) acrylate, decyl (meth) acrylate, isodecyl (meth) acrylate, undecyl (meth) acrylate, dodecyl (meth) acrylate, lauryl (meth) acrylate, stearyl (meth) acrylate, Alkyl (meth) acrylates such as isostearyl (meth) acrylate; hydroxyethyl (meth) acrylate, 2-hydroxypropyl (meth) acrylate, Rokishipuropiru (meth) acrylate, 2-hydroxybutyl (meth) acrylate, 3
Hydroxyalkyl (meth) acrylates such as -hydroxybutyl (meth) acrylate and 4-hydroxybutyl (meth) acrylate; phenoxyethyl (meth)
Phenoxyalkyl (meth) acrylates such as acrylate and 2-hydroxy-3-phenoxypropyl (meth) acrylate; 2-methoxyethyl (meth) acrylate, 2-ethoxyethyl (meth) acrylate, 2
-Alkoxyalkyl (meth) acrylates such as propoxyethyl (meth) acrylate, 2-butoxyethyl (meth) acrylate and 2-methoxybutyl (meth) acrylate; polyethylene glycol mono (meth) acrylate, ethoxydiethylene glycol (meth) acrylate, methoxy Polyethylene glycol (meth) acrylate, phenoxy polyethylene glycol (meth) acrylate, nonylphenoxy polyethylene glycol (meth) acrylate, polypropylene glycol mono (meth) acrylate, methoxypolypropylene glycol (meth) acrylate, ethoxypolypropylene glycol (meth) acrylate, nonylphenoxy Polyalkylenes such as polypropylene glycol (meth) acrylate Recol (meth) acrylate; cyclohexyl (meth) acrylate, 4-butylcyclohexyl (meth) acrylate, dicyclopentanyl (meth) acrylate, dicyclopentenyl (meth) acrylate, dicyclopentadienyl (meth) acrylate, bornyl ( Examples thereof include cycloalkyl (meth) acrylates such as (meth) acrylate, isobornyl (meth) acrylate, and tricyclodecanyl (meth) acrylate; benzyl (meth) acrylate, and tetrahydrofurfuryl (meth) acrylate. Among these, in the above general formula (I), the group represented by R ² is preferably a group containing an alkyl group or an oxyalkylene group, and a particularly preferred (meth) acrylate compound is methyl (meth) acrylate. Butyl (meth) acrylate, ethylhexyl (meth) acrylate, lauryl (meth) acrylate, isodecyl (meth) acrylate and 2-ethoxyethyl (meth) acrylate. The other copolymerizable monomer is not particularly limited as long as it is a compound copolymerizable with the above (meth) acrylate compound. For example, (meth) acrylic acid, vinyl benzoic acid, maleic acid, vinyl phthalic acid, etc. Unsaturated carboxylic acids; vinylbenzyl methyl ether, vinyl glycidyl ether,
Examples include a vinyl group-containing radically polymerizable compound such as styrene, α-methylstyrene, butadiene, and isoprene. In the acrylic resin constituting the composition of the present invention,
The content of the copolymer component derived from the (meth) acrylate compound represented by the general formula (I) is usually 70% by weight or more, preferably 90% by weight or more, and more preferably 100% by weight.

The molecular weight of the acrylic resin constituting the composition of the present invention is preferably 4,000 to 300,000, more preferably 10,000 to 20, as a weight average molecular weight in terms of polystyrene by GPC.
0000. The content of the binder resin in the composition of the present invention is preferably 5 to 40 parts by weight, more preferably 10 to 30 parts by weight, based on 100 parts by weight of the glass powder. If the ratio of the binder resin is too small, the glass powder cannot be securely bound and held.On the other hand, if the ratio is too large, a long time is required for the firing step or formation. The resulting glass sintered body (dielectric layer) may not have sufficient strength and film thickness.

<Solvent> The present invention is characterized in that a specific solvent is contained as a solvent constituting the composition. (1) The standard boiling point (boiling point at 1 atm) of the specific solvent is 1
The temperature is set to 100 to 200 ° C, preferably 110 to 180 ° C. When the standard boiling point of the specific solvent exceeds 200 ° C., the boiling point of the whole contained solvent is too high, and when a glass paste composition containing such a solvent is applied to produce a transfer film. In addition, a considerable amount of organic solvent remains in the film-forming material layer of the obtained transfer film, and a blocking phenomenon is likely to occur when the transfer film is wound up in a roll and stored. On the other hand, when the standard boiling point of the specific solvent is lower than 100 ° C., the boiling point of the entire solvent is too low, and an agglomerate of glass powder is generated in the glass paste composition containing such a solvent. The film-forming material layer formed by applying the composition is liable to generate film defects such as streaky coating marks, craters, and pinholes.

(2) The vapor pressure of the specific solvent at 20 ° C. is 0.5 to 50 mmHg, preferably 0.7 to 30 mmHg.
mmHg. If the vapor pressure of the specific solvent at 20 ° C. is less than 0.5 mmHg, the vapor pressure of the contained solvent as a whole is too low, and the glass paste composition containing such a solvent is applied. When a transfer film is manufactured, a considerable amount of an organic solvent remains in the film forming material layer of the obtained transfer film, and a blocking phenomenon is likely to occur when the transfer film is wound up in a roll and stored. On the other hand, when the vapor pressure of the specific solvent at 20 ° C. exceeds 50 mmHg, the vapor pressure of the entire solvent becomes too high, and the glass paste composition containing such a solvent has a quick drying property and is coated. The leveling property at the time is insufficient, and the uniformity of the film thickness tends to deteriorate.

(3) The surface tension of the specific solvent at 20 ° C. is preferably 25 dyn / cm or more. When the surface tension of the specific solvent at 20 ° C. is less than 25 dyn / cm, the surface tension of the contained solvent becomes low, and a glass paste composition containing such a solvent is applied to form a film. When a material layer is formed, a glass sintered body (dielectric layer) formed by firing the film forming material layer may become cloudy and may not have sufficient transparency (light transmittance). is there.

The specific solvent constituting the composition of the present invention satisfies the above conditions (1) and (2), and preferably satisfies the above condition (3), of ketones, alcohols and esters. Selected from among.

Specific examples of the specific solvent include ketones such as diethyl ketone, methyl butyl ketone, dipropyl ketone and cyclohexanone; and n-pentanol, 4-methyl-2-pentanol, cyclohexanol and diacetone alcohol. Alcohols; 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 monocarbonates such as n-butyl acetate and amyl acetate Carboxylic acid alkyl esters; ethyl lactate, lactic acid-
Lactic acid esters such as n-butyl; methyl cellosolve acetate, ethyl cellosolve acetate, propylene glycol monomethyl ether acetate, ethyl-3-
Examples thereof include ether esters such as ethoxypropionate. Of these, methyl butyl ketone, cyclohexanone, diacetone alcohol, ethylene glycol monobutyl ether, propylene glycol monomethyl ether, ethyl lactate, and ethyl-3-
Ethoxypropionate and the like are preferred. These specific solvents can be used alone or in combination of two or more.

The solvent other than the specific solvent which may be contained in the composition of the present invention has good affinity (dispersibility) with the glass powder, solubility of the binder resin, and good compatibility with the specific solvent. The glass paste composition can be given an appropriate viscosity together with the specific solvent, and can be selected from those which can be easily evaporated and removed by drying. Specific examples of such solvents include turpentine, ethyl cellosolve, methyl cellosolve, terpineol, butyl carbitol acetate,
Examples thereof include butyl carbitol, isopropyl alcohol, and benzyl alcohol.

In the composition of the present invention, the ratio of the specific solvent to the total solvent is usually 50% by weight or more, preferably 70% by weight or more. In addition, the content of the solvent (specific solvent and other solvents) in the composition of the present invention, from the viewpoint of maintaining the viscosity of the composition in a suitable range, based on 100 parts by weight of glass powder,
It is preferably 5 to 50 parts by weight, more preferably 10 to 40 parts by weight.

The glass paste composition of the present invention contains, in addition to the above essential components, a dispersant, a tackifier, a plasticizer,
Various additives such as a surface tension modifier, a stabilizer, and an antifoaming agent may be contained as optional components. As an example of a preferred glass paste composition, as a glass powder, 100 parts by weight of a mixture composed of 50 to 80% by weight of lead oxide, 5 to 20% by weight of boron oxide, and 10 to 30% by weight of silicon oxide, and polybutyl methacrylate ( Acrylic resin)
Examples of the composition include 30 parts by weight and 10 to 50 parts by weight of propylene glycol monomethyl ether (specific solvent) as essential components.

The composition of the present invention is prepared by kneading the above-mentioned glass powder, binder resin, solvent and optional components using a kneader such as a roll kneader, a mixer, a homomixer, a ball mill, a bead mill and the like. Can be. The composition of the present invention prepared as described above is a paste-like composition having fluidity suitable for application,
The viscosity is usually from 1,000 to 30,000 cp, preferably from 3,000 to 10,000 cp.

The composition of the present invention can be suitably used for producing a transfer film. This transfer film is a composite material composed of a support film and a film-forming material layer formed on the support film, and applied to a dry film method.

The supporting film constituting the transfer film includes:
It is preferable that the resin film has heat resistance and solvent resistance and is flexible. Since the support film has flexibility, the composition of the present invention can be applied by a roll coater, a blade coater, or the like, and the film-forming material layer is stored in a rolled state,
Can be supplied. As the resin forming the support film, for example, polyethylene terephthalate, polyester, polyethylene, polypropylene, polystyrene,
Polyimide, polyvinyl alcohol, polyvinyl chloride,
Examples thereof include fluorine-containing resins such as polyfluoroethylene, nylon, and cellulose. The thickness of the support film is, for example, 20 to 100 μm.

The film forming material layer constituting the transfer film includes:
Applying the composition of the present invention on the support film, drying the coating film to remove part or all of the solvent (for example,
(Until the solvent content becomes 0 to 1.0% by weight).

The method of applying the composition of the present invention on a supporting film is a method capable of efficiently forming a large (eg, 20 μm or more) coating film having excellent thickness uniformity. Specific examples include a coating method using a roll coater, a coating method using a blade coater, a coating method using a curtain coater, and a coating method using a wire coater. The surface of the support film to which the composition of the present invention is applied is preferably subjected to a release treatment. Thereby, in the step of transferring to the glass substrate, the operation of peeling the support film can be easily performed. Further, the transfer film may be provided with a protective film layer on the surface of the film forming material layer. Examples of such a protective film layer include a polyethylene terephthalate film, a polyethylene film, and a polyvinyl alcohol-based film. A film-forming material layer formed by applying the composition of the present invention on a support film (a film-forming material layer constituting a transfer film) has excellent flexibility (roll processability) due to containing an acrylic resin, And it has excellent adhesion to a glass substrate.

As described above, the composition of the present invention can be suitably used for producing a transfer film by forming a film-forming material layer on a support film, but is limited to these uses. Instead, a method for forming a film-forming material layer conventionally known, that is, the composition is directly applied to the surface of a glass substrate by a screen printing method or the like, and the film is dried to form a film-forming material layer. The method can also be suitably used.

[0033]

Hereinafter, embodiments of the present invention will be described.
The present invention is not limited by these. In the following, “parts” indicates “parts by weight”. Preparation of <Example 1> (1) Glass paste composition: as glass powder, lead oxide 60 wt%, boron oxide 10 _{wt%, PbO-B 2 O 3} -Si having a composition of silicon oxide 30 wt%
Acrylic resin (polystyrene conversion by GPC) obtained by copolymerizing 100 parts of an O ₂ -based mixture (softening point: 550 ° C.) and butyl methacrylate (70% by weight) and methyl methacrylate (30% by weight) as a binder resin (Weight average molecular weight: 80,000) and 20 parts of methyl butyl ketone (specific solvent) as a solvent were kneaded using a disperser to prepare a composition of the present invention having a viscosity of 7,000 cp.

(2) Production of transfer film: A support film (400 mm wide, 30 m long, 38 μm thick) made of polyethylene terephthalate (PET) which has been pre-released from the composition of the present invention prepared in the above (1). ) Was applied using a blade coater.
The solvent was removed by drying at 5 ° C. for 5 minutes, thereby producing a transfer film having a 50 μm-thick film-forming material layer formed on a support film.

(3) Evaluation of transfer film: The content of the solvent (methyl butyl ketone) remaining in the film forming material layer of the transfer film manufactured in the above (2) was determined by gas chromatography. % By weight or less, and no stickiness was observed on the surface of the film forming material layer. Further, when the surface state of the film-forming material layer was observed using a microscope, no film defects such as agglomerates of glass powder, streaky coating marks, craters and pinholes were observed. Further, this transfer film is
The test piece was cut into a size of 10 cm × 10 cm to prepare 10 test pieces, and the test pieces were superimposed to form a laminate. The laminate was subjected to a compressive load (20 gf / cm ² ) on both sides, and then subjected to constant temperature After standing for 24 hours in a constant humidity environment (temperature: 40 ° C., relative humidity: 60%), the test pieces were peeled off from the laminate one by one. As a result, the test pieces could be easily peeled off, and no blocking phenomenon was observed.

(4) Transfer of the film forming material layer: manufactured in the above (2) so that the surface of the film forming material layer is brought into contact with the surface of the glass substrate for a 20-inch panel (the fixed surface of the bus electrode). The transfer films thus obtained were overlapped, and the transfer film was thermocompression-bonded with a heating roll. Here, as the pressing conditions, the surface temperature of the heating roll is 110 ° C., and the roll pressure is 3 k.
g / cm ² , and the moving speed of the heating roll was 1 m / min.
After the completion of the thermocompression bonding, the support film was peeled off from the film forming material layer. As a result, the film-forming material layer was transferred to and adhered to the surface of the glass substrate.

(5) Firing the film-forming material layer (forming the dielectric layer): The glass substrate on which the film-forming material layer was transferred and formed by the above (4) was placed in a firing furnace, and the temperature in the furnace was set to room temperature. To 560 ° C at a rate of 10 ° C / min.
By baking for 30 minutes in the temperature atmosphere, a dielectric layer made of a glass sintered body was formed on the surface of the glass substrate.

(6) Evaluation of dielectric layer: The thickness (average thickness and tolerance) of this dielectric layer was measured to be 30 μm ±
The thickness was in the range of 0.5 μm, and the uniformity of the film thickness was excellent. Further, five panel materials made of a glass substrate having a dielectric layer were prepared in this way, and the light transmittance (measurement wavelength: 600 nm) of the formed dielectric layer was 80%. It was confirmed that the composition had excellent transparency.

<Examples 2 to 4> A glass paste composition of the present invention was prepared in the same manner as in Example 1 except that the composition of the solvent was changed according to the formulation shown in Table 1. Next, a transfer film was produced in the same manner as in Example 1 except that each of the obtained glass paste compositions was used. After that, the transfer of the film-forming material layer and the baking treatment of the film-forming material layer were performed in the same manner as in Example 1 except that each of the obtained transfer films was used, and the dielectric layer ( (Thickness: 30 μm ± 0.5 μm). Evaluation results of the transfer film (content of solvent in the film forming material layer, stickiness on the surface of the film forming material layer, blocking phenomenon of the transfer film, presence / absence of a film defect in the film forming material layer) and light of the formed dielectric layer Table 1 shows the transmittance.

Comparative Example 1 A glass paste composition for comparison was prepared in the same manner as in Example 1 except that 20 parts of isopropyl alcohol was used in place of methyl butyl ketone (specific solvent) according to the formulation shown in Table 1. Was prepared, and a transfer film was produced using the glass paste composition. In the obtained transfer film, the content of the solvent (isopropyl alcohol) in the film forming material layer was 1% by weight or less, and no stickiness was observed on the surface of the film forming material layer. No blocking phenomenon was observed in the transfer film laminate. However, a large number of glass aggregates of about 20 to 50 μm were observed on the surface of the film-forming material layer, and streak-like coating traces and craters generated in the nuclei of the aggregates were also observed.
Next, the transfer of the film-forming material layer and the baking treatment of the film-forming material layer were performed in the same manner as in Example 1 except that the transfer film was used, and a dielectric layer (thickness: 30 μm ±) was formed on the surface of the glass substrate. 1.5 μm), and the light transmittance of the dielectric layer was measured to be 50%, which was inferior in transparency. The above results are summarized in Table 1.

Comparative Example 2 A glass paste composition for comparison was prepared in the same manner as in Example 1 except that 20 parts of diethylene glycol monobutyl ether was used in place of methyl butyl ketone (specific solvent) in accordance with the formulation shown in Table 1. An article was prepared, and a transfer film was manufactured using the glass paste composition. Observation of the surface state of the film-forming material layer of the obtained transfer film revealed no film defects such as agglomerates of glass powder, streaky coating marks, craters and pinholes. However, the content of the solvent (diethylene glycol monobutyl ether) in the film forming material layer was as high as 11% by weight, and stickiness was observed on the entire surface of the film forming material layer. In addition, the test piece could not be peeled off from the laminate of the transfer film prepared for confirming the presence or absence of the blocking phenomenon. Next, the transfer of the film-forming material layer and the baking treatment of the film-forming material layer were performed in the same manner as in Example 1 except that the transfer film was used, and a dielectric layer (thickness: 30 μm ± 0.5 μm), and the light transmittance of the dielectric layer was measured to be 82%.
The above results are summarized in Table 1.

[0042]

[Table 1]

[0043]

According to the composition of the present invention, the following effects can be obtained. (1) A film-forming material layer having a low solvent content can be formed by low-temperature and short-time drying. (2) Since a specific solvent having an excellent affinity for glass powder is contained, no aggregate of glass powder is formed in the composition. (3) It is possible to form a film forming material layer excellent in uniformity without film defects. (4) A film-forming material layer having excellent flexibility can be formed. (5) A film-forming material layer having excellent adhesion to a glass substrate can be formed. (6) A dielectric layer having a high light transmittance can be formed. (7) It can be suitably used for the production of a transfer film. (8) A transfer film having excellent blocking resistance can be manufactured. (9) A transfer film having excellent roll processability can be manufactured.

[Brief description of the drawings]

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

[Explanation of symbols]

 DESCRIPTION OF SYMBOLS 1 Glass substrate 2 Glass substrate 3 Partition wall 4 Bus electrode 5 Address electrode 6 Phosphor 7 Dielectric layer 8 Protective layer

 ────────────────────────────────────────────────── ─── Continued from the front page (72) Inventor Atsushi Kumano 2--11-24 Tsukiji, Chuo-ku, Tokyo Inside Nippon Gosei Rubber Co., Ltd.

Claims (1)

[Claims] 1. A glass powder, (B) a binder resin, and (C) at least one selected from ketones, alcohols and esters satisfying the following conditions (1) and (2): A glass paste composition comprising: an organic solvent. Condition (1): The standard boiling point is 100 to 200 ° C. Condition (2): vapor pressure at 20 ° C. is 0.5 to 50 mm
Hg.