JPH1171132A - Glass paste composition - Google Patents

Abstract

PROBLEM TO BE SOLVED: To obtain a composition capable of forming a dielectric layer having high light transmission without containing baking residue even when a film forming material layer formed is subjected to baking treatment at a relatively low temperature by including glass powder, a binder component consisting essentially of a binder resin and a solvent and specifying a prescribed weight loss temperature of the binder component. SOLUTION: Glass powder having 400-600 deg.C softening point is preferable as the glass powder. Example of the glass powder includes a mixture of lead oxide with boron oxide and silicon oxide. The temperature of a binder component in 95% weight loss is <=350 deg.C. An acrylic resin, e.g. copolymer of butyl methacrylate with 2-ethoxyethyl methacrylate is preferable as the binder resin. The binder component content is 10-30 pts.wt. based on 100 pts.wt. glass powder. The weight average molecular weight of the binder resin is preferably 10,000-150,000. A ketone, an alcohol or an ester whose standard boiling points is 100-200 deg.C are used as the solvent and the content of the solvent is 5-50 pts.wt. based on 100 pts.wt. glass powder.

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 component essential for a binder resin, and a solvent is prepared, and this glass paste composition is prepared. A film-forming material layer is formed by coating and drying the surface of the glass substrate 1 by a screen printing method, and then the film-forming material layer is baked to remove a binder component (organic substance) and to remove the glass powder. Is known. Here, as the binder resin constituting the glass paste composition, methylcellulose, ethylcellulose, cellulose derivatives such as carboxymethylcellulose, polyvinyl alcohol, polyvinyl butyral, polyethylene glycol, urethane-based resin, melamine-based resin and the like are known, Among these, the dispersibility of the glass powder,
Ethyl cellulose is considered to be preferable from the viewpoints of the coating properties of the composition, the easiness of combustion, etc.
-31619).

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 to be about 1.3 to 2.0 times the thickness,
For example, in order to set the thickness of the dielectric layer 7 to 20 to 50 μm, it is necessary to form a film forming material layer having a thickness of about 30 to 100 μm. 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.

[0004] However, when the film forming material layer is formed 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 problem in forming a film-forming material layer by a screen printing method, the present inventors applied a glass paste composition on a supporting film, dried the coating film, and dried 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 method of forming a dielectric layer on a surface of a substrate (hereinafter, referred to as “dry film method”) has been proposed (see Japanese Patent Application No. 8-196304). Here, as an example of the transfer step in the dry film method, a composite film (hereinafter, referred to as “transfer film”) in which a film-forming material layer is formed on a support film is placed on the surface (electrode fixing surface) of a glass substrate. After the superposition, the heating roller is moved on the transfer film so that the film forming material layer is heated and adhered to the surface of the glass substrate, and then the support film is transferred from the film forming material layer adhered and fixed to the surface of the glass substrate. Can be mentioned. According to the PDP manufacturing method including such a dry film method, it is possible to form a dielectric layer having excellent film thickness uniformity and surface uniformity. Further, according to this manufacturing method, it is advantageous in that the transfer film, which is a material for forming the dielectric layer, can be wound into a roll and stored.

[0006]

However, when a glass paste composition containing a conventionally known resin such as a cellulose derivative is applied onto a support film to form a film-forming material layer (to produce a transfer film), Since the film forming material layer constituting the transfer film does not have sufficient adhesiveness (heat adhesiveness) to the glass substrate, there is a problem that it is difficult to transfer the film from the support film to the surface of the glass substrate. In order to solve such a problem, the present inventors have prepared a glass paste composition containing an acrylic resin such as polybutyl methacrylate, and applied the glass paste composition onto a support film to form a film-forming material. It has been found that a transfer film having excellent transferability of the layer (adhesion of the film-forming material layer to the glass substrate by heating) can be obtained.

On the other hand, when a film forming material layer formed on a glass substrate is fired, a binder component (organic substance such as a binder resin) constituting the film forming material layer is not completely decomposed and removed. In the formed dielectric layer (sintered glass), a residue derived from an organic substance (hereinafter, also referred to as a "baked residue").
Is included. Such a firing residue is particularly likely to be contained when a glass powder having a low softening point is used (when the firing temperature is low) or when polyvinyl butyral or a cellulose derivative is used as a binder resin. The light transmission of the layer may be impaired.

The present invention has been made based on the above circumstances. A first object of the present invention is to provide a glass paste composition that can form a glass sintered body containing no firing residue even by a firing process performed at a relatively low temperature (for example, 500 ° C. or lower). It is in. A second object of the present invention is to form a dielectric layer having a high light transmittance, which does not contain a firing residue, by firing a formed film forming material layer at a relatively low temperature. It is to provide a glass paste composition.
A third object of the present invention is to provide a glass paste composition that can be suitably used for producing a transfer film. A fourth object of the present invention is to provide a glass paste composition capable of producing a transfer film excellent in transferability of a film-forming material layer (heat adhesion of the film-forming material layer to a glass substrate). .

[0009]

The glass paste composition of the present invention comprises [A] a glass powder, [B] a binder component essential for a binder resin, and [C] a solvent. B]
The 95% weight loss temperature of the binder component is 350 ° C. or less.

In the glass paste composition of the present invention, the following embodiments are preferred. (1) 80% of the binder resin constituting the binder component [B]
Weight loss temperature is 300 ° C or less. (2) As the binder resin constituting the [B] binder component,
Acrylic resin must be contained. (3) As the binder resin constituting the [B] binder component,
A homopolymer of an alkoxyalkyl (meth) acrylate compound and / or a copolymer containing an alkoxyalkyl (meth) acrylate compound as a monomer component are contained.

[0011]

BEST MODE FOR CARRYING OUT THE INVENTION Hereinafter, the glass paste composition of the present invention will be described in detail. The glass paste composition of the present invention contains [A] glass powder, [B] a binder component, and [C] a solvent.

<Glass powder> Constituting the composition of the present invention
As a glass powder, its softening point is 400-600 ° C.
Those within the range are preferred. Softening point of glass powder is 4
When the temperature is lower than 00 ° C., a film forming material using the composition
In the sintering step of the binder layer, the binder component (such as binder resin)
Glass powder is not completely decomposed and removed
Organic substances in the formed dielectric layer due to melting
And fired residues, resulting in the dielectric layer being colored.
Light transmittance tends to decrease. On the other hand, the softness of the glass powder
If the conversion point exceeds 600 ° C,
Due to the necessity of firing, distortion etc. occurs on the glass substrate.
Easy to grow. Specific examples of suitable glass powder include:
Lead oxide, boron oxide, silicon oxide (PbO-B_TwoO_Three−
SiO_TwoSystem), zinc oxide, boron oxide, acid
Silicon oxide (ZnO-B_TwoO_Three-SiO_TwoMixture),
 Lead oxide, boron oxide, silicon oxide, aluminum oxide
(PbO-B_TwoO_Three-SiO_Two-Al_TwoO_ThreeSystem)
Compound, lead oxide, zinc oxide, boron oxide, silicon oxide
(PbO-ZnO-B _TwoO_Three-SiO_TwoSystem)
And the like.

<Binder Component> The "binder component" constituting the composition of the present invention comprises a "binder resin" as an essential component and an "additive" as an optional component. The composition of the present invention is characterized in that a 95% weight loss temperature of a binder component constituting the composition is 350 ° C. or less. By defining the 95% weight loss temperature of the binder component at 350 ° C. or lower, a relatively low firing temperature (for example, 500 ° C. or lower) is set as the firing condition of the film forming material layer containing the binder component. Also, it is possible to form a dielectric layer having a high light transmittance that does not include a firing residue.

<Binder Resin (Indispensable Component of Binder Component)> As the binder resin constituting the binder component, a glass powder can be bound with an appropriate degree of tackiness, and it has excellent thermal decomposability. Is required. Here, from the viewpoint of forming a glass sintered body (dielectric layer) containing no firing residue, the 80% weight loss temperature of the binder resin is preferably 300 ° C. or less. The binder resin having such excellent thermal decomposability (low-temperature decomposability) can be obtained, for example, by using a (meth) acrylate compound (particularly, alkoxyalkyl (meth) acrylate) described later as a monomer component. Can be prepared. That is, an acrylic resin can be mentioned as a preferred binder resin constituting the composition of the present invention. Acrylic resin has excellent thermal decomposability (low-temperature decomposability), and the film-forming material layer containing the acrylic resin exhibits excellent (heat) adhesion to a glass substrate. As a result, in the case where the composition of the present invention is applied to a support film to produce a transfer film, the resulting transfer film has excellent transferability of the film-forming material layer (transferability to a glass substrate). Becomes Such acrylic resin includes a homopolymer of a (meth) acrylate compound represented by the following general formula (1), a copolymer of two or more (meth) acrylate compounds represented by the following general formula (1), And a copolymer of a (meth) acrylate compound represented by the following general formula (1) and another copolymerizable monomer. The above-mentioned copolymer constituting the acrylic resin may be any of a random copolymer, a block copolymer, a graft copolymer, and an alternating copolymer.

[0015]

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

Specific examples of the (meth) acrylate compound represented by the general formula (1) include methyl (meth) acrylate, ethyl (meth) acrylate, propyl (meth) acrylate, isopropyl (meth) acrylate, and butyl ( (Meth) acrylate, isobutyl (meth)
Acrylate, t-butyl (meth) acrylate, pentyl (meth) acrylate, amyl (meth) acrylate, isoamyl (meth) acrylate, hexyl (meth) acrylate, heptyl (meth) acrylate, octyl (meth) acrylate, isooctyl (meth) Acrylate, 2-ethylhexyl (meth) acrylate, nonyl (meth) acrylate, decyl (meth) acrylate, isodecyl (meth) acrylate, undecyl (meth) acrylate, dodecyl (meth) acrylate, tridecyl (meth) acrylate, lauryl (meth) Acrylate, stearyl (meth) acrylate,
Alkyl (meth) acrylates such as isostearyl (meth) acrylate; hydroxymethyl (meth) acrylate, 2-hydroxyethyl (meth) acrylate, 2-hydroxypropyl (meth) acrylate, 3
Hydroxyalkyl (meth) acrylates such as -hydroxypropyl (meth) acrylate, 2-hydroxybutyl (meth) acrylate, 3-hydroxybutyl (meth) acrylate, and 4-hydroxybutyl (meth) acrylate; ethylene glycol monomethyl (meth) acrylate (Meth) acrylates having a hydroxyl group such as ethylene glycol monoethyl (meth) acrylate and glycerol (meth) acrylate; 2-methoxyethyl (meth) acrylate, 2-ethoxyethyl (meth) acrylate, 2-propoxyethyl (meth) ) Acrylate, 2-butoxyethyl (meth) acrylate,
Examples thereof include alkoxyalkyl (meth) acrylates such as 2-methoxybutyl (meth) acrylate. Among them, the alkoxyalkyl (meth) acrylate can be obtained as a monomer component (co).
The polymer is particularly preferable because it has excellent thermal decomposability (low-temperature decomposability). In the (co) polymer, it is preferable that the (co) polymer component derived from alkoxyalkyl (meth) acrylate is contained in an amount of 10% by weight or more.

The other copolymerizable monomer to be copolymerized with the (meth) acrylate compound is not particularly limited as long as it is a compound copolymerizable with the (meth) acrylate compound. ) Unsaturated carboxylic acids such as acrylic acid, vinyl benzoic acid, maleic acid and vinyl phthalic acid; and vinyl group-containing radically polymerizable compounds such as vinyl benzyl methyl ether, vinyl glycidyl ether, styrene, α-methyl styrene, butadiene and isoprene. be able to. In the acrylic resin used as the binder resin, the copolymer component derived from the (meth) acrylate compound represented by the general formula (1) generally has a content of 70%.
% By weight, preferably 90% by weight or more, more preferably 100% by weight.

Here, acrylic resins suitable as the binder resin include copolymers of butyl methacrylate and 2-ethoxyethyl methacrylate, copolymers of butyl methacrylate and 2-ethylhexyl methacrylate, and butyl methacrylate and 2-hydroxy methacrylate. Examples thereof include a copolymer with propyl methacrylate. The molecular weight of the binder resin constituting the composition of the present invention may be GP
The weight average molecular weight in terms of polystyrene by C (elution solvent: THF) is preferably 10,000 to 150,000, and more preferably 40,000 to 100000.
0000.

The content of the binder resin in the composition of the present invention is 10 to 100 parts by weight of the glass powder.
It is preferably 30 parts by weight, more preferably 1 part by weight.
5 to 25 parts by weight. If the proportion of the binder resin is too small, the glass powder cannot be bound and held reliably. On the other hand, if this ratio is excessive, a long time is required for the firing step, or the formed glass sintered body (dielectric layer) may not have sufficient surface smoothness.

<Additives (Optional Components of Binder Component)> Examples of additives that are optional components of the binder component include dispersants, tackifiers, plasticizers, surface tension regulators, stabilizers, and defoamers. , Dispersants and the like. The amount of the additive to be used is set so that the excellent thermal decomposability of the binder component (low-temperature decomposability at a 95% weight loss temperature of 350 ° C. or less) is not impaired.

<Solvent> The solvent constituting the composition of the present invention has a good affinity for glass powder and a good solubility of the binder component, and can impart an appropriate viscosity to the glass paste composition. In addition, it is preferable that the material can be easily evaporated and removed by drying. As a particularly preferred solvent, the standard boiling point (boiling point at 1 atm) is 10
Ketones, alcohols and esters having a temperature of 0 to 200 ° C. (hereinafter, these are referred to as “specific solvents”) can be exemplified. Specific examples of such a specific solvent include ketones such as diethyl ketone, methyl butyl ketone, dipropyl ketone and cyclohexanone; alcohols such as n-pentanol, 4-methyl-2-pentanol, cyclohexanol and diacetone alcohol Ether ethers 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 acids such as n-butyl acetate and amyl acetate Alkyl esters; lactate esters such as ethyl lactate and n-butyl lactate; methyl cellosolve acetate, ethyl cellosolve acetate;
Propylene glycol monomethyl ether acetate,
Examples thereof include ether esters such as ethyl-3-ethoxypropionate.
Methyl butyl ketone, cyclohexanone, diacetone alcohol, ethylene glycol monobutyl ether, propylene glycol monomethyl ether, ethyl lactate,
Ethyl-3-ethoxypropionate and the like are preferred.
These specific solvents can be used alone or in combination of two or more. Specific examples of the solvent other than the specific solvent include turpentine, ethyl cellosolve, methyl cellosolve, terpineol, butyl carbitol acetate, butyl carbitol, isopropyl alcohol,
Benzyl alcohol and the like can be mentioned. As the content ratio of the solvent in the composition of the present invention, from the viewpoint of maintaining the viscosity of the composition in a suitable range, the glass powder 100
The amount is preferably 5 to 50 parts by weight, more preferably 10 to 40 parts by weight with respect to parts by weight. The content ratio of the specific solvent to all solvents is 50% by weight.
Or more, more preferably 70% by weight.
That is all.

As an example of a preferred glass paste composition, as a glass powder, 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
100 parts by weight of butyl methacrylate / 2-ethoxyethyl methacrylate copolymer (copolymerization ratio: 80/20) as binder resin, and 10 to 30 parts by weight;
Propylene glycol monomethyl ether 1 as solvent
A composition containing 0 to 50 parts by weight as an essential component can be mentioned. The composition of the present invention comprises the above glass powder, a binder component (a binder resin and an additive that is an optional component).
In addition, the solvent can be prepared by kneading using a kneader such as a roll kneader, a mixer or a homomixer. The composition of the present invention prepared as described above is a paste-like composition having fluidity suitable for application.

The composition of the present invention can be particularly preferably 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 used in a process of forming a dielectric layer by a dry film method. Here, the viscosity of the glass paste composition (the composition of the present invention) to be subjected to the step of applying to the support film by the dry film method is preferably from 1,000 to 20,000.

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

The film forming material layer constituting the transfer film comprises:
The composition can be formed by applying the composition of the present invention on the support film, drying the coating film and removing a part or all of the solvent. As a method of applying the composition of the present invention on a support film, it is preferable that a method can efficiently form a large (for example, 20 μm or more) coating film having excellent thickness uniformity, Specifically, a coating method using a roll coater, a coating method using a blade coater, a coating method using a curtain coater, a coating method using a wire coater, and the like can be preferably mentioned. 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.

As described above, the composition of the present invention can be particularly preferably used in producing a transfer film by forming a film-forming material layer on a support film, but is not limited to these uses. Instead, a conventionally known method for forming a film-forming material layer, 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. Here, it is preferable that the viscosity of the glass paste composition (the composition of the present invention) to be subjected to the step of coating the glass substrate by the screen printing method is 10,000 to 200,000.

[0027]

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 a glass powder, lead oxide 70 wt%, boron oxide 20 _{wt%, PbO-B 2 O 3} -Si having a composition of silicon oxide 10 wt%
Acrylic resin [GPC obtained by copolymerizing 100 parts of an O ₂ -based mixture (softening point: 450 ° C.) and butyl methacrylate (80% by weight) and 2-ethoxyethyl methacrylate (20% by weight) as a binder resin Weight average molecular weight in terms of polystyrene by using: 85,000, thermogravimetric analysis /
Differential thermal analysis (hereinafter, also referred to as “TG / DTA”. Measurement device: TG / DTA300 manufactured by Seiko Instruments Inc.)
80% weight loss temperature: 260 ° C.] and kneading 23 parts of propylene glycol monomethyl ether as a solvent using a dispersing machine to give a viscosity of 3,500.
A composition of the invention was prepared that was 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 subjected to a release treatment from the composition of the present invention prepared in the above (1). ) Was applied using a roll coater to form a uniform coating film on the surface of the support film. Next, the formed coating film was dried at 100 ° C. for 5 minutes to remove the solvent, thereby producing a transfer film having a 30 μm-thick film-forming material layer formed on a support film.

(3) Evaluation of transfer film: The film forming material layer of the transfer film produced in the above (2) was evaluated for TG /
When the 95% weight loss temperature of the binder component was measured by DTA, it was 320 ° C. When the surface state of the film-forming material layer was observed using a microscope, no film defects such as aggregates of glass powder, streaky coating marks, craters, and pinholes were found.

(4) Transfer of the film forming material layer: manufactured in the above (3) such 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 is transferred and formed by the above (4) is placed in a firing furnace, and the temperature in the furnace is set to room temperature. To 570 ° 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 the dielectric layer was measured to be 15 μm ±
The thickness was in the range of 1 μm, and the film thickness was excellent in uniformity. Further, when this dielectric layer was visually observed, no firing residue derived from the binder component was observed.
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 85 to 95%. And had good colorless transparency.

<Example 2> Butyl methacrylate / 2-
Butyl methacrylate (60% by weight) instead of acrylic resin made of ethoxyethyl methacrylate copolymer
Resin obtained by copolymerization of 2-ethylhexyl methacrylate (40% by weight) [polystyrene-equivalent weight average molecular weight by GPC: 60,000, TG
A composition of the present invention having a viscosity of 2,300 cp was prepared in the same manner as in Example 1 except that 23 parts of a / 80% weight loss temperature by DTA was used. The composition of the present invention thus obtained is applied on a support film similar to that used in Example 1 by using a roll coater to form a uniform coating film on the surface of the support film. did. Next, the formed coating film was heated to 100 ° C.
For 5 minutes to remove the solvent, thereby producing a transfer film having a 30 μm-thick film-forming material layer formed on a support film. With respect to the film forming material layer of the transfer film thus obtained, the temperature at which the binder component was reduced by 95% by TG / DTA was measured.
42 ° C. Further, when the surface state of the film-forming material layer was observed using a microscope, aggregates of glass powder,
No film defects such as streak-like paint marks, craters and pinholes were found. The transfer film manufactured as described above is superimposed on the surface of the glass substrate for a 20-inch panel (the surface on which the bus electrode is fixed) so that the surface of the film-forming material layer is in contact with the glass substrate. The transfer film was thermocompression-bonded by a heating roll under the pressure-bonding conditions, and then 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. The glass substrate on which the film-forming material layer was transferred and formed as described above was placed in a firing furnace, and was baked under the same conditions as in Example 1. A body layer was formed. When the film thickness (average film thickness and tolerance) of this dielectric layer was measured, it was in the range of 15 μm ± 1 μm, and the film had excellent uniformity in film thickness. Further, when this dielectric layer was visually observed, no firing residue derived from the binder component was observed. 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 85 to 95%. And had good colorless transparency.

<Comparative Example 1> Butyl methacrylate / 2-
Ethyl cellulose [Wako Pure Chemical Industries, Ltd.] in place of the acrylic resin consisting of ethoxyethyl methacrylate copolymer
The same procedure as in Example 1 was carried out, except that 23 parts of 55 cp, viscosity (50 g / l, 25 ° C.), ethoxy group content of 45 to 50%, 80% weight loss temperature by TG / DTA: 353 ° C.) were used. A composition having a viscosity of 200,000 cp was prepared. The composition thus obtained was applied on a support film similar to that used in Example 1 using a roll coater to form a uniform coating film on the surface of the support film. Next, the formed coating film was dried at 100 ° C. for 5 minutes to remove the solvent, thereby producing a transfer film having a 30 μm-thick film forming material layer formed on a support film. With respect to the film forming material layer of the transfer film thus obtained, TG
When the 95% weight loss temperature of the binder component was measured by / DTA, it was 460 ° C. When the surface state of the film-forming material layer was observed using a microscope, no film defects such as aggregates of glass powder, streaky coating marks, craters, and pinholes were found. The transfer film manufactured as described above is superimposed on the surface of the glass substrate for a 20-inch panel (the surface on which the bus electrode is fixed) so that the surface of the film-forming material layer is in contact with the glass substrate. Depending on the pressure bonding conditions, this transfer film is thermocompressed with a heating roll,
Thereafter, 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. The glass substrate on which the film-forming material layer was transferred and formed as described above was placed in a baking furnace, and was baked under the same conditions as in Example 1.
A dielectric layer made of a glass sintered body was formed on the surface of the glass substrate. Thickness of this dielectric layer (average thickness and tolerance)
Was found to be in the range of 15 μm ± 1 μm, indicating that the film thickness was excellent in uniformity. In addition, when this dielectric layer was visually observed, a firing residue derived from the binding component was observed. Further, in this manner, five panel materials made of a glass substrate having a dielectric layer were prepared, and the light transmittance (measurement wavelength: 600 n) of the formed dielectric layer was prepared.
m) was 50 to 70% when measured, and the transparency was impaired by the firing residue.

[0035]

According to the composition of the present invention, the following effects can be obtained. (1) Even in a baking treatment performed at a relatively low temperature (for example, 500 ° C. or lower), it is possible to form a glass sintered body that does not include a baking residue. (2) Even when the formed film forming material layer is fired at a relatively low temperature, it is possible to form a dielectric layer containing no fired residue and having high light transmittance. The dielectric layer can be suitably used as a component of a PDP. (3) It can be suitably used for the production of a transfer film. (4) Transferability of film forming material layer (transferability to glass substrate)
It is possible to produce a transfer film excellent in quality.

[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 composition comprising [A] glass powder, [B] a binder component essential for a binder resin and [C] a solvent, wherein the 95% weight loss temperature of the [B] binder component is 350 ° C. A glass paste composition characterized by the following.