WO2012132651A1 - Composition de pâte, et procédé de production d'écran à plasma - Google Patents

Composition de pâte, et procédé de production d'écran à plasma Download PDF

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Publication number
WO2012132651A1
WO2012132651A1 PCT/JP2012/054224 JP2012054224W WO2012132651A1 WO 2012132651 A1 WO2012132651 A1 WO 2012132651A1 JP 2012054224 W JP2012054224 W JP 2012054224W WO 2012132651 A1 WO2012132651 A1 WO 2012132651A1
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Prior art keywords
glass powder
mass
paste
viscosity
paste composition
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PCT/JP2012/054224
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English (en)
Japanese (ja)
Inventor
井口雄一朗
小林康宏
山本洋平
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東レ株式会社
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Application filed by 東レ株式会社 filed Critical 東レ株式会社
Priority to KR1020137016957A priority Critical patent/KR20130139320A/ko
Priority to JP2012513106A priority patent/JPWO2012132651A1/ja
Publication of WO2012132651A1 publication Critical patent/WO2012132651A1/fr

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    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J9/00—Apparatus or processes specially adapted for the manufacture, installation, removal, maintenance of electric discharge tubes, discharge lamps, or parts thereof; Recovery of material from discharge tubes or lamps
    • H01J9/24—Manufacture or joining of vessels, leading-in conductors or bases
    • H01J9/241—Manufacture or joining of vessels, leading-in conductors or bases the vessel being for a flat panel display
    • H01J9/242—Spacers between faceplate and backplate
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J9/00—Apparatus or processes specially adapted for the manufacture, installation, removal, maintenance of electric discharge tubes, discharge lamps, or parts thereof; Recovery of material from discharge tubes or lamps
    • H01J9/02—Manufacture of electrodes or electrode systems
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J11/00—Gas-filled discharge tubes with alternating current induction of the discharge, e.g. alternating current plasma display panels [AC-PDP]; Gas-filled discharge tubes without any main electrode inside the vessel; Gas-filled discharge tubes with at least one main electrode outside the vessel
    • H01J11/10—AC-PDPs with at least one main electrode being out of contact with the plasma
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J11/00—Gas-filled discharge tubes with alternating current induction of the discharge, e.g. alternating current plasma display panels [AC-PDP]; Gas-filled discharge tubes without any main electrode inside the vessel; Gas-filled discharge tubes with at least one main electrode outside the vessel
    • H01J11/20—Constructional details
    • H01J11/34—Vessels, containers or parts thereof, e.g. substrates
    • H01J11/36—Spacers, barriers, ribs, partitions or the like
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J2211/00—Plasma display panels with alternate current induction of the discharge, e.g. AC-PDPs
    • H01J2211/20—Constructional details
    • H01J2211/34—Vessels, containers or parts thereof, e.g. substrates
    • H01J2211/36—Spacers, barriers, ribs, partitions or the like
    • H01J2211/366—Spacers, barriers, ribs, partitions or the like characterized by the material

Definitions

  • the present invention relates to a paste composition.
  • the present invention relates to a paste suitable for forming an insulating pattern used for a flat display such as a plasma display panel, a field emission display, and a fluorescent display tube, and a method for manufacturing a flat display panel.
  • the plasma display generates plasma discharge between the electrodes facing each other in the discharge space provided between the front glass substrate and the rear glass substrate, and is generated from the gas sealed in the discharge space. Display is performed by irradiating the phosphor provided in the discharge space with ultraviolet rays.
  • a gas discharge type display such as a plasma display or a fluorescent display tube requires an insulating partition for partitioning a discharge space.
  • a field emission display such as a field emission display requires an insulating partition for isolating the gate electrode from the cathode.
  • barrier rib paste is repeatedly applied in a pattern by a screen printing plate, dried and then screen printed by baking, masked with a resist on the dried barrier rib material layer, and sandblasted.
  • the sand blasting method for firing the dried partition wall material is fired, the layer is masked with a resist, and the etching method for etching (Patent Document 1), and the coating film of the partition wall paste has a pattern
  • a mold transfer method imprint method in which baking is performed (Patent Document 4)
  • a partition material made of a photosensitive paste material is applied, dried, exposed and developed.
  • a photosensitive paste method (photolithographic method) for performing baking is known (Patent Documents 2 and 5).
  • the organic substances are distilled off by combustion or decomposition in a high-temperature baking process, and then the glass is partially melted.
  • -It is a point which forms the pattern by an inorganic material by sintering.
  • the firing temperature is generally set to 650 ° C. or lower in order to suppress deformation of the glass substrate.
  • the above-described method has a problem in that when the organic component is removed by baking, stress acts and pattern defects are likely to occur.
  • the cause of the pattern defect is firstly the firing stress when the organic substance is fired and distilled at a high temperature, and secondly the shrinkage stress when the glass component is softened and shrunk at a high temperature.
  • Patent Document 3 suppresses pattern defects by increasing the strength of the pattern against stress by adding a urethane compound having excellent flexibility to the organic component.
  • a method has been proposed. This method is effective for preventing defects due to stress that occurs during the process of decomposition of organic matter during firing. However, after organic matter is removed by firing, the pattern due to shrinkage stress in the sintering process of glass components. There is no effect of deterring deficiencies.
  • the present invention is a paste that can suppress pattern defects that occur when inorganic materials are sintered by controlling the viscosity characteristics of glass materials at high temperatures, particularly by designing the amount of change in viscosity with respect to temperature within a certain range. Is to provide.
  • the present invention has the following configuration.
  • a low-melting-point glass powder comprising a glass powder and an organic component, the viscosity ⁇ 1 (dPa ⁇ s) at 570 ° C. and the viscosity ⁇ 2 (dPa ⁇ s) at 590 ° C. satisfying the following formula (1) Containing 40% by mass or more based on the total glass powder. 0.5 ⁇ log ⁇ 1-log ⁇ 2 ⁇ 0.9
  • (2) A paste composition containing glass powder and an organic component, wherein the glass powder has a viscosity ⁇ 1 (dPa ⁇ s) at 570 ° C.
  • a paste composition comprising a low melting point glass powder satisfying at least 40% by mass based on the total glass powder. 1.05 ⁇ log ⁇ 1 / log ⁇ 2 ⁇ 1.11 (2) (3) The paste composition according to (1) or (2), wherein the ⁇ 1 (dPa ⁇ s) and ⁇ 2 (dPa ⁇ s) satisfy the following formulas (3) and (4): 8.5 ⁇ log ⁇ 1 ⁇ 9.0 (3) 7.8 ⁇ log ⁇ 2 ⁇ 8.5 (4) (4) The paste composition as described in any one of (1) to (3) above, wherein the softening temperature of the low melting glass powder is 560 to 610 ° C.
  • Alkali metal oxide content X (M 2 O) (mass%) and zinc oxide content X (ZnO) (mass%) in the low melting glass powder satisfy the following formula (5), and Silicon oxide content X (SiO 2 ) (mass%), aluminum oxide content X (Al 2 O 3 ) (mass%) and boron oxide content X (B 2 O 3 ) ( Mass%) satisfying the following formula (6), the content X (M 2 O) of the alkali metal oxide in the low-melting glass powder is in the range of 4 to 10 mass%, and zinc oxide
  • the paste of the present invention it is possible to obtain an inorganic pattern having no defect after firing, and in particular, it is possible to provide a display member having no defect in the pattern, which is effective for manufacturing a low-cost, high-yield PDP. It is.
  • the paste of the present invention is composed of an organic substance and an inorganic powder.
  • a certain amount of organic matter is required to form a pattern before firing, but if there are too many organic components, the amount of substances removed in the firing step increases and the firing shrinkage ratio increases, so the firing step Pattern defects are likely to occur.
  • organic substances are likely to remain in the baking process, and the remaining organic substances are likely to cause contamination in the display.
  • the organic component is too small, not only the mixing and dispersion of inorganic fine particles in the paste will be insufficient, but also problems such as a decrease in paste applicability due to an increase in paste viscosity will result in a stable paste. There are also adverse effects on the properties, which may be undesirable.
  • the content of inorganic fine particles in the paste is preferably 40% by mass to 80% by mass, and more preferably 40% by mass to 70% by mass.
  • a glass powder having a softening temperature of 480 ° C. or higher as the low-melting glass powder to be used in order to remove organic substances almost completely by firing and to ensure a certain strength.
  • the softening temperature is 480 ° C. or lower, the glass is softened before the organic components are sufficiently removed during firing, and the organic residue is taken into the glass. In this case, there is a concern that the organic matter is gradually released later and the product quality is deteriorated. Therefore, after patterning a paste using glass powder with a softening temperature of 480 ° C. or higher, heating it to 500 ° C.
  • the firing temperature is 620 ° C. or higher, the deformation is increased in a general glass substrate. Therefore, the firing temperature is preferably 620 ° C. or lower. That is, for the formation of the inorganic material pattern in the display, it is desirable to bake at 500 to 620 ° C. As a characteristic of the low melting point glass powder in the paste used at this time, glass having a softening temperature of 480 to 620 ° C. is used. Is preferred.
  • the baking shrinkage tends to occur in a short time, the instantaneous shrinkage stress tends to increase, and the pattern defect tends to occur. Therefore, by making the change in the viscosity of the low-melting glass powder in this high temperature region constant, firing shrinkage can be moderately performed, and pattern defects due to shrinkage stress can be made difficult to occur. In particular, it is important to keep the viscosity fluctuation in the region of 570 to 590 ° C. below a certain level. That is, by using a low-melting glass powder having a viscosity ⁇ 1 (dPa ⁇ s) at 570 ° C.
  • the viscosity ⁇ 1 (dPa ⁇ s) at 570 ° C. and the viscosity ⁇ 2 (dPa ⁇ s) at 590 ° C. of the low softening point glass can be measured using a penetration method described later.
  • log ⁇ 1 -log ⁇ 2 If the value of log ⁇ 1 -log ⁇ 2 is 0.5 or less, softening due to heating becomes difficult to proceed sufficiently. That is, low softening point glass sintered by heating generally has log ⁇ 1 -log ⁇ 2 larger than 0.5. On the other hand, if it is 0.9 or more, the change in viscosity with respect to temperature is large, and pattern defects due to instantaneous contraction stress are likely to occur.
  • the softening temperature is 560 to 610 ° C.
  • moderate sintering proceeds and an inorganic pattern having excellent strength can be formed.
  • the softening temperature as used in the present invention can usually be measured using a differential thermal analyzer (DTA).
  • DTA differential thermal analyzer
  • the endothermic end temperature at the endothermic peak is determined by the tangent method. It can be obtained by extrapolation.
  • the content of the low melting point glass contained in the paste composition of the present invention is required to be 40% by mass or more based on the total glass powder in terms of sinterability.
  • strength after baking can be formed by containing 40 mass% or more of low melting glass powder which has the relationship of following formula (3) and (4).
  • log ⁇ 1 and log ⁇ 2 satisfy the above formulas (3) and (4). If log ⁇ 1 or log ⁇ 2 is too large, sintering is difficult to proceed and the strength of the formed product may be insufficient. On the other hand, when log ⁇ 1 or log ⁇ 2 is too small, the pattern shape may be deformed together with the glass sintering, and the shape retention may be difficult. That is, by making the range satisfying the above formula, a particularly appropriate sinterability can be obtained, and an inorganic pattern having no defects can be obtained.
  • the low softening point glass powder contained in the paste composition of the present invention can use lead oxide, bismuth oxide, zinc oxide and alkali metal oxides, which are effective materials for lowering the melting point of glass.
  • Lead oxide is undesirable in the environment, and bismuth oxide is disadvantageous in that it uses expensive element bismuth. Therefore, it is desirable to adjust the softening temperature of the glass using an alkali metal oxide.
  • the alkali metal refers to lithium, sodium, potassium, rubidium, and cesium.
  • the alkali metal oxide contained as a constituent of the low softening point glass powder of the present invention includes lithium oxide, sodium oxide, and potassium oxide. The total content of lithium oxide, sodium oxide and potassium oxide is X (M 2 O).
  • the content X (M 2 O) of the alkali metal oxide is preferably 4 to 10% by mass in the whole glass. If it is less than 4% by mass, the softening temperature may not be sufficiently reduced for firing on a glass substrate. Moreover, when more than 10 mass%, the viscosity at high temperature may fall too much. Furthermore, the viscosity at high temperature is too low by adjusting the softening temperature with an alkali metal alone. Therefore, it is desirable to add 3 to 10% by mass of zinc oxide. If it is less than 3% by mass, the viscosity at high temperature is high, and if it is more than 10% by mass, the cost of the glass tends to be high.
  • the alkali metal oxide content X (M 2 O) (mass%) and the zinc oxide content X (ZnO) (mass%) in the low melting glass powder satisfy the following formula (5). Desirable from the point of control. 1.0 ⁇ X (M 2 O) / X (ZnO) ⁇ 3.0 (5) It is desirable from the viewpoint of high temperature viscosity control that X (M 2 O) / X (ZnO) is designed to be in the range of 1.0 to 3.0. If it is less than 1.0, the high-temperature viscosity becomes too high, and if it is more than 3.0, it becomes too low.
  • the low melting point glass includes oxides of silicon oxide, boron oxide, aluminum oxide, alkaline earth metals (magnesium, calcium, barium, strontium, etc.) in addition to the above alkali metal oxides and lead oxides. By using it, the stability, crystallinity, transparency, thermal expansion characteristics, etc. of the glass can be controlled.
  • a low-melting-point glass having viscosity characteristics used in the present invention can be produced by using the following composition.
  • the alkaline earth metal indicates one or more selected from magnesium, calcium, barium, and strontium.
  • the silicon oxide content X (SiO 2 ) (mass%), the aluminum oxide content X (Al 2 O 3 ) (mass%), and the boron oxide content X (B 2 O 3 ) (mass%) preferably satisfies the following formula (6).
  • Boron oxide is effective in improving the flow characteristics of glass at high temperatures, but conversely, it tends to change the fluidity and viscosity with respect to temperature.
  • silicon oxide or aluminum oxide reduces fluidity at high temperatures, but has the effect of reducing the change in viscosity with respect to temperature. Therefore, by satisfying the above relationship, a change in viscosity with respect to temperature can be appropriately maintained while maintaining fluidity at high temperatures.
  • oxides selected from titanium oxide, zirconium oxide, bismuth oxide, and various metal oxides can be added, but these oxides are preferably less than 10% by mass. If added in an amount of 10% by mass or more, there is a problem that the properties of the glass are impaired or the cost is increased due to discoloration or crystallization.
  • the viscosity characteristic at high temperature of the low softening point glass powder used in the present invention is measured using the “penetration method” for measuring the viscosity (medium viscosity range) when the glass is softened and sintered. it can.
  • the measuring device can measure using a high temperature penetration type viscometer (product number: PVM-1400) manufactured by Opto.
  • PVM-1400 high temperature penetration type viscometer manufactured by Opto.
  • the viscosity can be determined by measuring the load applied by the load cell. In actual measurement, the penetration indenter is pushed into the surface of the flat glass sample at a constant penetration speed, and the viscosity is measured by the following formula from the load applied to the penetration rod.
  • the 50% volume average particle size (D50) is in the range of 1.0 to 4.0 ⁇ m. If it is less than 1.0 ⁇ m, the aggregation of particles becomes strong, it becomes difficult to obtain uniform dispersibility, and the fluidity of the paste becomes unstable. In such a case, the thickness uniformity when the paste is applied decreases. On the other hand, when D50 exceeds 4.0 ⁇ m, the surface unevenness of the sintered body becomes large, which tends to cause the pattern to be crushed in a subsequent process.
  • the paste composition of the present invention may contain high melting point glass that does not soften even at 650 ° C. or ceramic particles such as silica, alumina, zirconia, etc. as filler components.
  • the filler can be used together with the low melting point glass in order to control the firing shrinkage rate and maintain the shape of the partition wall to be formed.
  • these fillers preferably have an average particle size of 0.5 to 4.0 ⁇ m for the same reason as in the low melting point glass.
  • various organic components can be used depending on the process for pattern processing.
  • celluloses such as ethyl cellulose and nitrocellulose are used as a binder, and terpineol is used as a solvent.
  • terpineol is used as a solvent.
  • a paste prepared using cellulose, butyral resin, acrylic resin and an organic solvent is applied and dried with a slit coater, a film resist is applied, and the resist film is applied by a photolithography method (pattern exposure / The pattern can be formed by a method of patterning using development and removing the resist-removed portion by sandblasting.
  • a more preferable processing method using the paste composition of the present invention is a photosensitive paste method using the paste composition of the present invention as a photosensitive paste containing a photoreactive material as an organic component.
  • the photosensitive paste can form a highly accurate pattern by photolithography after being applied and dried on the substrate.
  • the stress until organic substance is baked and distilled off can be relieve
  • deletion can be suppressed.
  • the refractive index of the organic substance and the inorganic substance is set at the time of light irradiation in order to increase the light transmittance. It is necessary to match and suppress light scattering.
  • As an organic component it is necessary to have the following relationship between the average refractive index n1 of the component remaining after distilling off the solvent component having a boiling point of 250 ° C. or less and the average refractive index n2 of the glass powder. -0.1 ⁇ n1-n2 ⁇ 0.1
  • the characteristics of glass components composed of various oxides can be controlled by considering their blending, and low melting point glass powders with controlled thermal characteristics, refractive index, etc. can also be used in the present invention.
  • the paste composition of the present invention includes a photoreactive material as an organic component, and can be a photosensitive paste that can be patterned by exposure and development.
  • the photoreactive material the reactivity can be controlled by adding a reactive monomer, a reactive oligomer, a photopolymerization initiator, or the like.
  • the reactivity in the reactive monomer and reactive oligomer means that when the paste is irradiated with actinic rays, the reactive monomer or reactive oligomer undergoes a reaction such as photocrosslinking or photopolymerization to cause a chemical structure. Means change.
  • the photosensitive monomer include compounds having an active carbon-carbon double bond, and monofunctional and polyfunctional compounds having a vinyl group, an acryloyl group, a methacryloyl group, and an acrylamide group as functional groups.
  • those containing 10 to 80 parts by weight of a polyfunctional acrylate compound and a methacrylate compound in the organic component are preferred from the viewpoint of increasing the crosslink density during curing by photoreaction and improving the pattern forming property. Since various types of compounds have been developed as the polyfunctional acrylate compound and methacrylate, it can be appropriately selected in consideration of reactivity, refractive index, and the like.
  • a paste material that is less prone to pattern loss can be obtained. This is because when the low melting point glass powder having the high-temperature viscosity characteristic of the present invention is used, it is difficult to cause rapid shrinkage in the process of sintering the glass in the latter stage of heating and firing, while suppressing pattern defects.
  • a compound having a urethane structure is used as the organic binder, the organic component in the initial stage of overheating is decomposed and distilled, that is, stress relaxation occurs in the overheating process in the state where the organic matter remains, resulting in pattern defects. This is due to a mechanism that is difficult to produce. By having both of these characteristics, pattern defects can be suppressed in a wide temperature range.
  • the paste composition of the present invention can contain a copolymer having a carboxyl group as a binder.
  • the copolymer having a carboxyl group include carboxyl group-containing monomers such as acrylic acid, methacrylic acid, itaconic acid, crotonic acid, maleic acid, fumaric acid, vinyl acetic acid, and acid anhydrides thereof, and methacrylic acid esters, acrylics, and the like. It is obtained by selecting monomers such as acid ester, styrene, acrylonitrile, vinyl acetate, 2-hydroxyacrylate and copolymerizing using an initiator such as azobisisobutyronitrile.
  • a copolymer having acrylic acid ester or methacrylic acid ester and acrylic acid or methacrylic acid as a copolymerization component is preferably used since the thermal decomposition temperature at the time of firing is low.
  • the paste By containing a carboxyl group, the paste is excellent in solubility in an alkaline aqueous solution, and development after pattern exposure becomes possible.
  • the acid value of the copolymer having a carboxyl group is preferably 50 to 150 mgKOH / g. By setting the acid value to 150 mgKOH / g or less, the development allowable range can be widened. Moreover, the solubility with respect to the developing solution of an unexposed part does not fall because an acid value shall be 50 mgKOH / g or more. Therefore, it is not necessary to increase the concentration of the developing solution, and peeling of the exposed portion can be prevented, and a high-definition pattern can be obtained.
  • the copolymer having a carboxyl group has an ethylenically unsaturated group in the side chain.
  • the ethylenically unsaturated group include an acryl group, a methacryl group, a vinyl group, and an allyl group.
  • the paste composition of the present invention comprises a glass powder and an organic component, an organic solvent and a binder as necessary (in the case of a photosensitive paste, in addition to these, a reactive monomer, a reactive oligomer, a reactive polymer, a photopolymerization initiator).
  • a photosensitive paste in addition to these, a reactive monomer, a reactive oligomer, a reactive polymer, a photopolymerization initiator.
  • the viscosity of the paste can be appropriately adjusted depending on the addition ratio of inorganic fine particles, thickener, organic solvent, plasticizer, anti-settling agent, etc., but the range is preferably in the range of 2 to 200 Pa ⁇ s.
  • a viscosity of 2 to 5 Pa ⁇ s is preferable.
  • a viscosity of 50 to 200 Pa ⁇ s is preferred.
  • a viscosity of 10 to 50 Pa ⁇ s is preferable.
  • a display member can be obtained by applying the paste of the present invention thus obtained on a substrate, forming a pattern using various methods, and further baking. Especially the paste of this invention can be used conveniently for manufacture of the plasma display member which has a partition on a board
  • a method for forming the pattern for example, a screen printing method, a sand blast method, a photolithography method, or the like can be used. Photolithography is preferable because high-definition processing is possible.
  • ⁇ Paste is applied to the entire surface or a part of the substrate to form a coating film.
  • a coating method methods such as a screen printing method, a bar coater, a roll coater, a die coater, and a blade coater can be used.
  • the coating thickness can be adjusted by selecting the number of coatings, screen mesh and paste viscosity.
  • a proximity exposure machine or the like can be used as the exposure apparatus.
  • a large area can be exposed with an exposure machine having a small exposure area by applying the paste on the substrate and then performing the exposure while transporting.
  • development is performed using the difference in solubility between the exposed portion and the unexposed portion of the coating film in the developer.
  • Development is performed by dipping, spraying, or brushing.
  • an organic solvent in which the organic components in the paste can be dissolved can be used. Further, water may be added to the organic solvent as long as its dissolving power is not lost.
  • the developer is preferably composed mainly of water.
  • development can be performed with an alkaline aqueous solution.
  • the alkaline aqueous solution sodium hydroxide, sodium carbonate, calcium hydroxide aqueous solution or the like can be used.
  • it is preferable to use an organic alkaline aqueous solution because an alkaline component can be easily removed during firing.
  • an aqueous solution of an inorganic alkali such as sodium carbonate, potassium carbonate, sodium hydroxide, or sodium bicarbonate can be used.
  • a general amine compound specifically examples include tetramethylammonium hydroxide, trimethylbenzylammonium hydroxide, monoethanolamine, and diethanolamine.
  • the concentration of the alkaline aqueous solution is usually 0.05 to 5% by mass, more preferably 0.1 to 1% by mass. If the alkali concentration is too low, the soluble portion is not removed, and if the alkali concentration is too high, the pattern portion may be peeled off and the non-soluble portion may be corroded.
  • the development temperature at the time of development is preferably 20 to 50 ° C. for process control.
  • firing is performed in a firing furnace.
  • the firing atmosphere and temperature vary depending on the type of paste and substrate, but firing is performed in an atmosphere of air, nitrogen, hydrogen, or the like.
  • As the firing furnace a batch-type firing furnace or a belt-type continuous firing furnace can be used.
  • Calcination is usually preferably performed by holding at a temperature of 480 to 610 ° C. for 10 to 60 minutes. Through the above steps, a display member in which a pattern made substantially of an inorganic material is formed on a substrate is obtained.
  • Examples 1 to 8, Comparative Examples 1 to 4 Comparative Examples 1 to 4.
  • the penetration indenter was pushed into the flat glass sample surface at a penetration speed of 0.1 mm / min (less than 550 ° C.) and 1.0 mm / min (more than 550 ° C.), and the viscosity was measured by the following formula from the load applied to the penetration rod.
  • ⁇ G ⁇ W / V ⁇ : viscosity, G: apparatus constant, W: load applied to the penetrating rod (g), V: penetration speed (mm / sec) D.
  • IC369 2-benzyl-2-d
  • Polymerization inhibitor 1,6-hexanediol-bis [(3,5-di-tert-butyl-4-hydroxyphenyl) propionate])
  • Ultraviolet absorber solution Sudan IV (manufactured by Tokyo Ohka Kogyo Co., Ltd.)
  • ⁇ -butyrolactone 0.3 mass% solution viscosity modifier Flownon EC121 (manufactured by Kyoeisha Chemical Co., Ltd.)
  • Solvent ⁇ -butyrolactone glass powder: Glass powders 1 to 6 shown in Table 1 were used.
  • the photosensitive pastes of Examples 1 to 6 and Comparative Examples 1 to 3 were prepared by the following method.
  • the glass powder shown in Table 2 was added to 60% by mass of the produced organic solution 1 or 2, and then kneaded with a three-roller kneader to produce a paste. Moreover, the back substrate for plasma displays was produced with the following method using the produced paste.
  • Striped address silver electrodes (line width 50 ⁇ m, thickness 3 ⁇ m, pitch 300 ⁇ m) are formed on a 42-inch diagonal glass substrate, and a dielectric layer 15 ⁇ m thick is formed thereon, and then the above paste was applied and dried to a dry thickness of 160 ⁇ m.
  • a photomask stripe pattern, line width 50 ⁇ m, pattern pitch 300 ⁇ m for the purpose of forming a barrier rib pattern for plasma display was set and exposed in an arrangement parallel to the address electrodes. After exposure, the film was developed in a 0.5% ethanolamine aqueous solution and further baked at 595 ° C. for 15 minutes.
  • a display member having stripe-shaped partition walls having a pitch of 300 ⁇ m, a line width of 50 ⁇ m, and a height of 120 ⁇ m could be obtained.
  • the pastes of Examples 7 and 8 and Comparative Example 4 were prepared by the following procedure.
  • An organic solution 3 was prepared by dissolving 3% by mass of ethyl cellulose resin and 5% by mass of dibutyl phthalate as a plasticizer in a solvent in which terpineol and diethylene glycol monobutyl ether acetate were mixed in a ratio of 1: 1.
  • the glass powder shown in Table 2 was added to 60% by mass of the solution, and then kneaded with a three-roller kneader to prepare a paste.
  • Striped address silver electrodes (line width 50 ⁇ m, thickness 3 ⁇ m, pitch 250 ⁇ m) are formed on a 42 inch diagonal glass substrate, and a dielectric layer 15 ⁇ m thick is formed thereon, and then the above paste was applied and dried to a dry thickness of 140 ⁇ m.
  • a negative drip film resist (Nippon Synthetic Chemical Industry Co., Ltd., NCP225, 25 ⁇ m) having a protective film was laminated with a hot roll at 100 ° C.
  • a line-and-space pattern mask having a pitch of 300 ⁇ m and an opening width of 50 ⁇ m is aligned and placed on the resist layer, irradiated with ultraviolet rays (364 nm, intensity of 20 mW / cm 2, irradiation amount of 120 mJ / cm 2), exposed to photo
  • the protective film on the resist layer was peeled off, and spray development was performed using a 1% by mass aqueous solution of sodium carbonate having a liquid temperature of 30 ° C.
  • a resist pattern corresponding to the line pattern mask was obtained.
  • the disconnection start size was evaluated by the following method.
  • a mask having 40 to 40 pattern defects each having a size of 5 to 40 ⁇ m formed (a light slit having a constant width is formed in the opening) is used.
  • % Of the pattern defects 40 pattern defects of the same size were produced in the mask, of which 20 were broken) were defined as the break start size.
  • This evaluation is an evaluation showing how easily a pattern defect is generated when a mask flaw is formed or a foreign substance adheres during the process, and the larger the value, the better.
  • Table 2 shows the evaluation results of the photosensitive pastes obtained in Examples 1 to 8 and Comparative Examples 1 to 4.
  • the present invention can be usefully used as a paste for forming a partition with a small amount of residual organic components. Further, a partition wall having a small amount of remaining organic components is formed, and it can be effectively used as a flat panel display with excellent display characteristics such as luminance and color purity and high panel reliability.

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  • Physics & Mathematics (AREA)
  • Plasma & Fusion (AREA)
  • Manufacturing & Machinery (AREA)
  • Glass Compositions (AREA)
  • Gas-Filled Discharge Tubes (AREA)

Abstract

La présente invention concerne un motif comprenant un matériau inorganique qui a été formé en suivant les étapes consistant à : modeler une pâte comprenant une substance organique et une substance inorganique ; soumettre le produit obtenu à une procédure de cuisson à température élevée afin de distiller et faire partir la substance organique par brûlage ou décomposition ; puis fondre/fritter partiellement le verre obtenu. Cependant, ce procédé est problématique du fait que des défauts de motif risquent de se former sous l'action d'une contrainte appliquée durant le retrait du composant organique par cuisson. L'invention concerne une composition de pâte comprenant une poudre de verre et un composant organique, et caractérisée en ce que la poudre de verre comprend, selon une quantité de 40 % en masse ou plus par rapport à la quantité totale de poudre de verre, une poudre de verre à bas point de fusion dont la viscosité (η1) (dPa·s) à 570 °C et la viscosité (η2) (dPa·s) à 590 °C satisfont à la formule (1) : 0,5 < logη1 - logη2 < 0,9 (1). Cette composition de pâte permet de former un motif ne présentant aucun défaut de motif.
PCT/JP2012/054224 2011-03-25 2012-02-22 Composition de pâte, et procédé de production d'écran à plasma WO2012132651A1 (fr)

Priority Applications (2)

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KR1020137016957A KR20130139320A (ko) 2011-03-25 2012-02-22 페이스트 조성물 및 플라즈마 디스플레이의 제조 방법
JP2012513106A JPWO2012132651A1 (ja) 2011-03-25 2012-02-22 ペースト組成物およびプラズマディスプレイの製造方法

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JP2011-067354 2011-03-25

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KR (1) KR20130139320A (fr)
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Publication number Priority date Publication date Assignee Title
CN112768112B (zh) * 2020-12-29 2023-08-01 深圳市沁园春科技有限公司 电子料浆及其制备方法

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH11349349A (ja) * 1998-06-02 1999-12-21 Nippon Electric Glass Co Ltd プラズマディスプレーパネル用ガラスペースト
JP2001210141A (ja) * 2000-01-31 2001-08-03 Murata Mfg Co Ltd 感光性ガラスペースト及びそれを用いた多層配線回路板の製造方法
JP2005135682A (ja) * 2003-10-29 2005-05-26 Taiyo Ink Mfg Ltd 焼成物パターン
WO2010113580A1 (fr) * 2009-03-31 2010-10-07 東レ株式会社 Elément d'écran plat et pâte pour la couche supérieure de la cloison de séparation de l'élément d'écran plat

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH11349349A (ja) * 1998-06-02 1999-12-21 Nippon Electric Glass Co Ltd プラズマディスプレーパネル用ガラスペースト
JP2001210141A (ja) * 2000-01-31 2001-08-03 Murata Mfg Co Ltd 感光性ガラスペースト及びそれを用いた多層配線回路板の製造方法
JP2005135682A (ja) * 2003-10-29 2005-05-26 Taiyo Ink Mfg Ltd 焼成物パターン
WO2010113580A1 (fr) * 2009-03-31 2010-10-07 東レ株式会社 Elément d'écran plat et pâte pour la couche supérieure de la cloison de séparation de l'élément d'écran plat

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