JP2005067959A - Method for manufacturing glass paste composition for forming dielectric glass layer and method for manufacturing plasma display panel using the glass paste composition - Google Patents

Abstract

<P>PROBLEM TO BE SOLVED: To provide a method for manufacturing a glass paste composition capable of forming a dielectric glass layer with while suppressing the occurrence of residual bubbles which causes the lowering of insulation resistant voltage and light transmittance, and a method for manufacturing a plasma display panel provided with the dielectric glass layer having homogeneity, high transparency, high reliability and high insulation resistant voltage. <P>SOLUTION: The glass paste composition for forming the dielectric glass layer is prepared through a 1st kneading process for mixing a prescribed quantity of glass powder with a prescribed quantity of a resin a part of which is dissolved in a solvent and kneading the mixture and a 2nd kneading process for diluting the kneaded material in the 1st kneading process with a plasticizer and the residual solvent and kneading again. The glass paste composition prepared by this way is applied to cover an electrode formed on the surface of the glass substrate to form a base film for forming a layer and the dielectric glass layer is formed by firing the base film for forming the layer. <P>COPYRIGHT: (C)2005,JPO&NCIPI

Description

  The present invention relates to a method for producing a glass paste composition capable of suitably producing a dielectric glass layer in a plasma display panel used as a high-precision and inexpensive thin large-screen color display device, and a plasma display using the same The present invention relates to a panel manufacturing method.

  Plasma display panels can be roughly classified into two types: AC type and DC type according to the driving method, and can be classified into two types: a surface discharge type and a counter discharge type. At present, AC-type and surface-discharge-type plasma displays occupy the mainstream because they can have a large screen with high definition and are easy to manufacture.

  In manufacturing the plasma display panel, first, various projections made of electrodes, partition walls, and the like are formed on a glass substrate to manufacture a front panel and a rear panel, respectively. As the arrangement, the surroundings are sealed, and an inert gas is sealed in a sealed space formed between the two panels. Finally, the process is performed through a process of assembling a control circuit and a chassis.

  Next, a configuration of a general AC type surface discharge type plasma display panel will be described with reference to the drawings. 1 is a partially broken perspective view of a plasma display panel having a general configuration, FIG. 2 is a cross-sectional view taken along line AA in FIG. 1, and FIG. 3 is a cross-sectional view taken along line BB in FIG. The surface side glass substrate 1 is made of a heat resistant glass for plasma display such as a soda glass substrate or a high strain point glass. On one surface (the lower surface in FIGS. 1 and 2) of this surface side glass substrate 1, silver or Cr— A plurality of pairs of display electrodes 4 are formed in which scanning electrodes 2 and sustaining electrodes 3 made of Cu-Cr are arranged in parallel with each other in parallel. A light shielding layer 5 is formed between the display electrodes 4 adjacent to each other. Scan electrode 2 and sustain electrode 3 are respectively composed of transparent electrodes 2a and 3a and buses 2b and 3b made of silver or the like electrically connected thereto.

  The plurality of pairs of display electrodes 4 are covered with a dielectric glass layer 6 formed on one surface of the front glass substrate 1. Further, an MgO film 7 is formed on the surface of the dielectric glass layer 6, and this MgO film functions as a protective film and a secondary electron emission film.

  On the other hand, a rear glass substrate 8 similar to the front glass substrate 1 is provided so as to face one surface of the front glass substrate 1. Address electrodes 10 are formed on the back glass substrate 8 facing the front glass substrate 1 in an arrangement perpendicular to the display electrodes 4 including the scan electrodes 2 and the sustain electrodes 3. The address electrodes 10 are covered with a dielectric glass layer 9 formed on the back glass substrate 8. On the dielectric glass layer 9, a plurality of stripe-like partition walls 11 are formed so as to be parallel to the address electrodes 10. A phosphor layer 12 is provided on the peripheral side surface of each partition wall 11 and the surface of the dielectric glass layer 9. Each of the dielectric glass layers 6 and 9 is an electrical insulator and functions as a capacitor for storing electric charges.

  The surface side glass substrate 1 and the back side glass substrate 8 are arranged so as to face each other with a predetermined gap, and the periphery is sealed, and a minute discharge space is formed in the sealed interior. Yes. Therefore, scan electrode 2, sustain electrode 3, and address electrode 10 are arranged to face each other with a minute discharge space in an arrangement perpendicular to each other. One gas or a mixed gas of two or more of helium, neon, argon, and xenon is sealed in the discharge space as a discharge gas. Further, as clearly shown in FIG. 3, the discharge space is partitioned into a plurality of display spaces by the partition walls 11, and the intersections of the display electrodes 4 and the address electrodes 10 facing each other through the respective display spaces are provided. A discharge cell 13 is formed. In the discharge cell 13 selected by the address electrode 10 among the plurality of discharge cells 13, a small-scale address discharge is first generated between the scan electrode 2 and the sustain electrode 3, and then the scan electrode 2 and the sustain electrode are generated. The main discharge is generated between the three, and the display of the plasma display panel is performed.

  Further, in each discharge cell 13, phosphor layers 12 are sequentially arranged one by one so as to be red, green, and blue, and the space between the discharge cells 13 is covered by the light shielding layer 5. The discharge at is not visible from the outside.

  In such a plasma display panel, when the display electrode 4 and the dielectric glass layer 6 are formed on the front side glass substrate 1 and the address electrode 10 and the dielectric glass layer 9 are formed on the back side glass substrate 8, respectively. The following steps are performed. That is, for the display electrode 4 and the address electrode 10, after an electrode film is formed by patterning by screen printing or the like, the electrode film is separately fired to form an electrode.

On the other hand, for the dielectric glass layers 6 and 9, conventionally, a manufacturing method using a screen printing method has been generally employed. However, since this manufacturing method has various drawbacks, As a production method of No. 9, a paste-like composition containing glass powder, a binder resin and a solvent is applied on a support film, and then the coating film is dried to form a film-forming material layer. A method of producing dielectric glass layers 6 and 9 by transferring a forming material layer onto the surface of a glass substrate on which an electrode is fixed and then firing is known (for example, see Patent Document 1).
JP-A-9-102273

  However, the dielectric glass layer for a plasma display panel manufactured by the above-described conventional method has drawbacks such as low transparency and easy dielectric breakdown due to many bubbles remaining in the film. . That is, in the conventional manufacturing method, a mixture obtained by mixing glass powder, a binder resin and a solvent for forming a predetermined composition is kneaded until a predetermined viscosity is obtained. In the paste-like composition, the glass powders agglomerate with each other at the time of kneading, so that the glass powder is not uniformly dispersed throughout, and tends to be unevenly distributed in the glass powder.

  Therefore, the dielectric glass layer obtained by firing the film-forming material layer formed by applying this paste-like composition on a glass substrate is due to the uneven distribution of glass powder and binder resin. In the firing step, the generation of residual bubbles cannot be sufficiently suppressed. As a result, the obtained dielectric glass layer cannot have high transparency due to the deterioration of optical properties due to the presence of residual bubbles and the occurrence of protrusions and the like, and a highly smooth surface cannot be obtained. . In addition, the dielectric glass layer is likely to crack on the surface when a voltage is applied due to voids generated inside due to residual bubbles. It will be in a state and will cause a problem that dielectric breakdown occurs.

  Accordingly, the present invention provides a method for producing a glass paste composition capable of forming a dielectric glass layer by suppressing the generation of residual bubbles that cause a reduction in dielectric strength and light transmittance, and a homogeneous, highly transparent and highly reliable method. It is an object of the present invention to provide a method for manufacturing a plasma display panel having a dielectric glass layer having high performance and high dielectric strength voltage.

  In order to achieve the above object, a method for producing a glass paste composition for forming a dielectric glass layer according to the present invention comprises a required amount of glass powder and a resin dissolved in a required amount of a solvent. A first kneading step of kneading the mixture, and a second kneading step of kneading again the kneaded material obtained by the first kneading step in a state diluted with a plasticizer and a remaining solvent. It is characterized by being manufactured after that.

  In this method for producing a glass paste composition for forming a dielectric glass layer, since the mixture in the first kneading step is only mixed with a certain amount of the solvent, a relatively high viscosity is obtained. Thus, the glass powders can be kneaded so that they are not agglomerated with each other and stirred with good dispersibility, so that the glass powders are evenly distributed throughout. In the second kneading step, the kneaded product obtained by diluting the kneaded product already kneaded with the remaining amount of the solvent and the plasticizer is kneaded again to produce a glass paste composition having a predetermined viscosity. In the glass paste composition thus obtained, the glass powder is uniformly distributed throughout.

  In the first and second kneading steps in the above invention, it is preferable to knead the material to be kneaded by using a kneading apparatus in which a plurality of stirring blades revolve while rotating. Thus, the material to be kneaded can be effectively stirred so as to homogenize the whole by a plurality of stirring blades that perform planetary motion that revolves while rotating, so that the glass powder can be more effectively dispersed. It can be distributed uniformly throughout.

  The method for producing a plasma display panel according to the present invention comprises applying the glass paste composition produced by the production method of the above invention to a state in which the electrode is coated on the surface of the glass substrate on which the electrode is formed, It is characterized by comprising a step of forming a layer forming element film and a step of forming a dielectric glass layer by firing the layer forming element film.

  In this plasma display panel manufacturing method, the layer forming element film to be baked in the baking step is formed using a glass paste composition in which the glass powder is uniformly distributed over the whole. When the film is baked, defects such as internal voids and surface cracks due to residual bubbles generated due to uneven distribution of the glass powder hardly occur, and a good smooth surface free from small protrusions can be obtained. Therefore, the dielectric glass layer produced through the above steps has good optical characteristics and high dielectric strength due to uniform dispersion of the glass powder and reduction of the amount of residual bubbles in the film.

  As the step of forming the layer forming element film in the above invention, a glass paste composition is applied on a support film that has been subjected to a release treatment in advance to form a coating film, and the coating film is dried to form the layer forming element. A step of forming a body film, a step of thermocompression-bonding a transfer film in which the element film for layer formation is formed on the support film to the surface of the glass substrate, and the support film from the thermocompression-transferred film It is preferable that the method includes a step of peeling and removing. As a result, the transfer film was formed by applying the glass paste composition to the support film, so that the glass paste composition was directly applied to the surface of the glass substrate to form a layer forming element film. Thus, a required layer forming element film can be easily and reliably formed with high accuracy.

  In the above invention, it is preferable to use a binder resin having physical properties of a glass transition temperature of 0 to 30 ° C. as the resin of the glass paste composition. Thereby, since the binder resin having the physical properties of the glass transition temperature of 0 to 30 ° C. has good flexibility, stretchability and strong adhesiveness, the layer forming element film is placed on the surface of the glass substrate. It can be transferred reliably.

  The plasma display panel manufactured by the manufacturing method of the present invention has a high reliability in which a dielectric glass layer as an electrode covering material can ensure a high dielectric strength voltage and a very high light transmittance. It becomes.

  As described above, according to the method for producing a glass paste composition for forming a dielectric glass layer according to the present invention, the mixture in the first kneading step is mixed with a part of the required amount of the solvent. Therefore, the glass powder can be kneaded in a state having a relatively high viscosity, so that the glass powders can be kneaded without agglomeration and with good dispersibility so that the glass powder is evenly distributed throughout. In the second kneading step, the kneaded product obtained by diluting the kneaded product already kneaded with the remaining amount of the solvent and the plasticizer is kneaded again to produce a glass paste composition having a predetermined viscosity. In the glass paste composition thus obtained, the glass powder is uniformly distributed throughout.

  Further, according to the method for manufacturing a plasma display panel according to the present invention, the layer forming element film to be fired in the firing step is formed using a glass paste composition in which the glass powder is uniformly distributed throughout. Therefore, when firing the layer forming element film, a good smooth surface is obtained in which defects such as internal voids and surface cracks due to residual bubbles generated due to uneven distribution of the glass powder hardly occur and there are no small protrusions. be able to. Therefore, the dielectric glass layer produced through the above steps has good optical characteristics and high dielectric strength due to uniform dispersion of the glass powder and reduction of the amount of residual bubbles in the film.

  Hereinafter, preferred embodiments of the present invention will be described in detail. In this embodiment, a glass paste composition which is a material for forming the dielectric glass layers 6 and 9 for a plasma display panel is manufactured through the following steps. That is, the glass paste composition is prepared using a required amount of glass powder, a resin, a plasticizer, and a solvent, respectively. First, the resin is dissolved in a part of the required amount of the solvent. A resin dissolved in a solvent and a required amount of glass powder are mixed. As said resin, the binder resin which has a physical property whose glass transition temperature is 0-30 degreeC is used.

  A mixture of the glass powder and a resin dissolved in a solvent is kneaded using a kneading apparatus 14 as shown in FIG. The kneading device 14 includes a bottomed cylindrical storage container 17 that stores a material to be kneaded, a rotary lid body 18 that is rotationally driven in contact with the opening of the storage container 17 so as to cover the opening, The rotating lid 18 has two types of stirring blades 19 and 20 that are rotatably mounted in a suspended state. The rotary lid 18 is rotated by transmitting a rotational force from a rotational drive source via a rotary shaft 21 connected to the rotary lid 18, and the two stirring blades 19 and 20 are integrally rotated, that is, revolved. Let On the other hand, the two types of stirring blades 19 and 20 are individually rotated while being rotated integrally with the rotary lid 18 by transmitting the rotational force from the rotation driving mechanism via the individual rotating shafts 22 and 23. In other words, it rotates. Therefore, the stirring blades 19 and 20 are revolved integrally with the rotary lid 18 while rotating individually, so that the kite also performs a planetary motion.

  The mixture of glass powder, resin, and solvent stored in the storage container 17 is kneaded with a relatively high viscosity because the solvent is only mixed in a part of the required amount. And by being effectively stirred so as to homogenize the whole by the two kinds of stirring blades 19 and 20 that perform planetary motion that is revolved while rotating, the glass powder does not agglomerate with each other, and The glass powder and the resin are kneaded with good dispersibility and uniformly distributed throughout.

  When the kneading step is completed, the remaining amount of solvent and plasticizer are inserted into the container 17 to dilute the kneaded product, and the diluted kneaded product is mixed with the two stirring blades 19 and 20. The glass paste composition having a predetermined viscosity is prepared by kneading again by planetary motion. The glass paste composition thus obtained has glass powder and resin distributed uniformly throughout.

  Next, the glass paste composition produced as described above is applied on the surface of the support film that has been previously subjected to the mold release treatment by using a die coat, so that a uniform film made of the glass paste composition is formed on the support film. A thick coating is formed. Thereafter, by drying the coating film at a predetermined temperature for a predetermined time, a part or all of the solvent is removed, and a layer forming element film that becomes an element body of the dielectric glass layers 6 and 9 to be formed is obtained. Form.

  Subsequently, the transfer film in which the layer forming element film is formed on the support film is formed on the electrode forming surface of the glass substrates 1 and 8 on which the predetermined electrodes 3 and 9 are formed in advance using silver or the like. The layers are stacked in such a manner that the element film for layer formation comes into contact therewith. In this state, the transfer film is thermocompression bonded onto the glass substrates 1 and 8 using a heating roll. The surface temperature of the heating roll, the roll pressure by the heating roll, the moving speed of the heating roll, and the preheating temperature of the glass substrates 1 and 8 are set to optimum values according to the glass paste composition to be used. . As a result, the layer forming element film is transferred and brought into close contact with the surfaces of the glass substrates 1 and 8. At this time, the binder resin selected as the resin and having physical properties of glass transition temperature of 0 to 30 ° C. has good flexibility, stretchability and strong adhesiveness. Transfer to the surfaces of the glass substrates 1 and 8 can be ensured. By providing the step of forming this transfer film, the required layer forming element film can be formed in comparison with the case of forming the layer forming element film by directly applying the glass paste composition to the surface of the glass substrate. It can be easily and reliably formed with high accuracy.

  Next, after peeling off and removing the support film from the layer forming element film, the layer forming element film transferred to the surfaces of the glass substrates 1 and 8 is baked at a predetermined temperature, thereby forming the layer forming element film. The resin, plasticizer, and residual organic materials contained therein are removed by decomposition, and only the glass powder, which is an inorganic substance, is melted and sintered. Thereby, dielectric glass layers 6 and 9 made of a glass sintered body are formed on the surfaces of the glass substrates 1 and 8.

  Since the layer forming element film to be fired in the firing step is formed using a glass paste composition in which the glass powder is uniformly distributed throughout, the glass powder is fired at the time of firing the layer forming element film. It is possible to obtain a good smooth surface in which defects such as internal voids and surface cracks due to residual bubbles generated due to the uneven distribution of the surface do not occur and no small protrusions are present. Therefore, the dielectric glass layers 6 and 9 manufactured through the above steps have good optical characteristics and high insulation withstand voltage due to uniform dispersion of the glass powder and reduction of the amount of remaining bubbles in the film. . Since it has been confirmed through experiments that such a good effect can be obtained, an example thereof will be specifically described below.

For example, lead glass powder having a softening point of about 570 ° C. (P60: 40 wt%, SiO ₂ : 15 wt%, B ₂ O ₃ : 20 wt%, BaO: 18 wt%, Al) ₂ O ₃ : 7% by weight) glass powder component (100 parts by weight), polymethyl methacrylate (15 parts by weight) as binder resin, dioctyl phthalate (8 parts by weight) as plasticizer, triene and acetic acid as solvents Various components were prepared using a one-to-one mixed solution (50 parts by weight) of ethyl so as to have a desired composition by the following method.

  The glass powder (100 parts by weight), the binder resin (15 parts by weight) and the mixed solvent (30 parts by weight) are mixed, and this mixture is kneaded for 30 minutes using the kneader 14 shown in FIG. The remaining mixed solvent (20 parts by weight) and a plasticizer (8 parts by weight) were added and diluted, and the diluted state was kneaded with the kneader 14 for 60 minutes to prepare a glass paste composition. In that case, the glass paste composition of Examples 1-5 was used as Examples 1-5 using the said binder resin from which glass transition temperature mutually differs from 0 degreeC, 5 degreeC, 10 degreeC, 20 degreeC, and 30 degreeC, respectively. Prepared. Separately from Examples 1 to 5, glass paste compositions of Comparative Examples 1 and 2 were prepared using a binder resin having glass transition temperatures of 40 ° C. and 50 ° C.

  Moreover, the glass paste composition of Comparative Example 3 was prepared as follows. That is, the glass powder (100 parts by weight), the binder resin (8 parts by weight) and the mixed solvent (30 parts by weight) were kneaded for 30 minutes using the kneader 14 shown in FIG. Part), a mixed solvent (20 parts by weight) and a plasticizer (8 parts by weight) were added and diluted, and the mixture was further kneaded with the kneader 14 for 60 minutes in the diluted state. At this time, the binder resin having a glass transition temperature of 5 ° C. was used.

  Furthermore, the glass paste composition of Comparative Example 4 was prepared as follows. That is, after kneading the glass powder (100 parts by weight), binder resin (10 parts by weight), mixed solvent (30 parts by weight) and plasticizer (8 parts by weight) for 30 minutes using the kneader 14 shown in FIG. The remaining binder resin (5 parts by weight) and a mixed solvent (20 parts by weight) were added and diluted, and the mixture was further kneaded with the kneader 14 in the diluted state for 60 minutes. At this time, the binder resin having a glass transition temperature of 5 ° C. was used.

By applying the glass paste compositions prepared in Examples 1 to 5 and Comparative Examples 1 to 4 on a support film made of polyethylene terephthalate (PET), which has been subjected to a release treatment in advance, using a die coat, a support film A transfer film in which a film-forming material layer having a film thickness of 60 μm is formed on a support film by forming a film with a uniform film thickness on the film and drying the film for 3 minutes at a temperature of 80 ° C. Produced. Each transfer film thus produced was thermocompression bonded onto a glass substrate having a thickness of 42 inches on which required electrodes were formed with silver (Ag) using a heating roll. The conditions at that time are a roll temperature of the heating roll of 80 ° C., a roll pressure of the heating roll of 10 kg / cm ² , a moving speed of the heating roll of 1 m 2 / min, and a preheating temperature of the glass substrate of 80 ° C. Each film-forming material layer in each transfer film thus formed was baked at a temperature of 590 ° C. to form a dielectric glass layer on the glass substrate. At this time, the thickness of the dielectric glass layer was 30 μm.

  Dielectric breakdown tests were performed on the dielectric glass layers of Examples 1 to 5 and Comparative Examples 1 to 4 formed as described above. In this dielectric breakdown test, an interval of 200 μm was placed on an aluminum plate, a rare gas (one-to-one mixed gas of helium and neon) was passed between them, the discharge electrode was the positive electrode, In addition, with an aluminum plate as a negative electrode, an AC voltage was applied up to 500 V, and the number of dielectric breakdowns was measured.

  Further, a film-forming material layer is formed only on a glass substrate without an electrode by the same method as described above, and the total light transmittance (%) and haze (%) representing the haze of the dielectric film alone (%) It measured using HM-150 made from Murakami Color Research Laboratory, and the value at the time of 550 nm was compared. The results are shown in Table 1.

  As is clear from Table 1, the dielectric glass layers of Examples 1 to 5 have a high total light transmittance and a low haze indicating haze, which is a barometer of the diffusion ratio of light transmitted through the layer. In addition to having excellent optical characteristics, the occurrence of defects due to residual bubbles is suppressed, so that a very good result having a high dielectric strength voltage can be obtained. Such a good result is obtained by kneading a mixture of a glass powder and a resin dissolved in a solvent in advance with a high viscosity, and kneading again in a state where a plasticizer and a solvent are added to the kneaded product and diluted. It was obtained by using the obtained glass paste composition. That is, since the glass paste composition has good dispersibility of the glass powder, the amount of bubbles remaining in the film after firing is reduced, and good optical characteristics and high dielectric strength voltage can be obtained. It is a thing.

  In addition, since the dielectric glass layers of Comparative Examples 1 and 2 formed using a glass paste composition that employs a binder resin having a physical property of which the glass transition temperature exceeds 30 ° C. are weak in adhesiveness of the binder resin, Transfer from the support film to the glass substrate was difficult. The glass powder, the binder resin, the plasticizer, the solvent, and the like can obtain the same effects as described above by appropriately changing according to the characteristics of the material.

1 is a partially broken perspective view showing a general configuration of a plasma display panel which is an object of the present invention. AA sectional view taken on the line AA of FIG. FIG. 3 is a sectional view taken along line BB in FIG. 1. The disassembled perspective view which shows the kneading apparatus used for the manufacturing method of the plasma display panel of this invention.

Explanation of symbols

DESCRIPTION OF SYMBOLS 1,8 Glass substrate 4,10 Electrode 6,9 Dielectric glass layer 14 Kneading apparatus 19,20 Stirring blade

Claims (6)

A first kneading step of mixing a required amount of glass powder and a resin dissolved in a part of the required amount of the solvent, and kneading the mixture;
A glass paste composition for forming a dielectric glass layer, which is prepared through a second kneading step in which the kneaded product obtained in the first kneading step is kneaded again in a state diluted with a plasticizer and a remaining solvent. Manufacturing method. The glass paste for forming a dielectric glass layer according to claim 1, wherein in the first and second kneading steps, the material to be kneaded is kneaded using a kneading device in which a plurality of stirring blades revolve while rotating. A method for producing the composition. The glass paste composition produced by the production method according to claim 1 or 2 is applied so as to cover the surface of the glass substrate on which the electrode is formed, thereby forming a layer forming element film. Process,
And a step of forming a dielectric glass layer by firing the layer forming element film. As a step of forming a layer forming elemental film, a glass paste composition is applied on a support film that has been subjected to a release treatment in advance to form a coating film, and this coating film is dried to form the layer forming elemental film. A step of forming, a step of thermocompression bonding a transfer film in which the element film for layer formation is formed on the support film to the surface of the glass substrate, and peeling and removing the support film from the thermocompression transfer film The manufacturing method of the plasma display panel of Claim 3 provided with the process to perform. The manufacturing method of the plasma display panel of Claim 4 using binder resin which has a physical property with a glass transition temperature of 0-30 degreeC as resin of a glass paste composition. A plasma display panel manufactured by the manufacturing method according to claim 3.

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