WO2011108115A1 - 有機el封着用無鉛ガラス材とこれを用いた有機elディスプレイ及び該ディスプレイの製造方法 - Google Patents
有機el封着用無鉛ガラス材とこれを用いた有機elディスプレイ及び該ディスプレイの製造方法 Download PDFInfo
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- WO2011108115A1 WO2011108115A1 PCT/JP2010/053670 JP2010053670W WO2011108115A1 WO 2011108115 A1 WO2011108115 A1 WO 2011108115A1 JP 2010053670 W JP2010053670 W JP 2010053670W WO 2011108115 A1 WO2011108115 A1 WO 2011108115A1
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- lead
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Images
Classifications
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- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05B—ELECTRIC HEATING; ELECTRIC LIGHT SOURCES NOT OTHERWISE PROVIDED FOR; CIRCUIT ARRANGEMENTS FOR ELECTRIC LIGHT SOURCES, IN GENERAL
- H05B33/00—Electroluminescent light sources
- H05B33/10—Apparatus or processes specially adapted to the manufacture of electroluminescent light sources
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C12/00—Powdered glass; Bead compositions
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C8/00—Enamels; Glazes; Fusion seal compositions being frit compositions having non-frit additions
- C03C8/02—Frit compositions, i.e. in a powdered or comminuted form
- C03C8/04—Frit compositions, i.e. in a powdered or comminuted form containing zinc
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C8/00—Enamels; Glazes; Fusion seal compositions being frit compositions having non-frit additions
- C03C8/24—Fusion seal compositions being frit compositions having non-frit additions, i.e. for use as seals between dissimilar materials, e.g. glass and metal; Glass solders
-
- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05B—ELECTRIC HEATING; ELECTRIC LIGHT SOURCES NOT OTHERWISE PROVIDED FOR; CIRCUIT ARRANGEMENTS FOR ELECTRIC LIGHT SOURCES, IN GENERAL
- H05B33/00—Electroluminescent light sources
- H05B33/02—Details
- H05B33/04—Sealing arrangements, e.g. against humidity
-
- H—ELECTRICITY
- H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
- H10K50/00—Organic light-emitting devices
- H10K50/80—Constructional details
- H10K50/84—Passivation; Containers; Encapsulations
- H10K50/842—Containers
- H10K50/8426—Peripheral sealing arrangements, e.g. adhesives, sealants
-
- H—ELECTRICITY
- H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
- H10K59/00—Integrated devices, or assemblies of multiple devices, comprising at least one organic light-emitting element covered by group H10K50/00
- H10K59/80—Constructional details
- H10K59/87—Passivation; Containers; Encapsulations
- H10K59/871—Self-supporting sealing arrangements
- H10K59/8722—Peripheral sealing arrangements, e.g. adhesives, sealants
Definitions
- the present invention relates to an organic EL sealing lead-free glass material used for sealing a display using an organic EL (electroluminescence) element, an organic EL display having a panel peripheral portion sealed with the lead-free glass material, and the organic EL display. It relates to the manufacturing method.
- the organic EL display has a parallel stripe-shaped lower electrode 2, an organic light emitting layer 3, and a lower electrode 2 on one side (inner surface) side of a glass EL element substrate 1 in order from the lower layer side.
- a parallel stripe-shaped upper electrode 4 is formed along a direction orthogonal to the EL element substrate 1, and a peripheral portion between the EL element substrate 1 and the sealing glass plate 5 disposed to face the EL element substrate 1 is sealed with a sealing layer 6. Yes.
- Such an organic EL display has a bright and high construct and excellent display recognizability, and can be configured to be extremely thin.
- an ultra-thin display having a total thickness of 1 mm or less for a small device such as a mobile phone or a digital camera.
- the whole can be made of a solid material and that the driving circuit is simplified by direct current drive.
- the probability of a sealing technique for blocking the organic EL element from the outside air has become a big issue.
- a sealing method using a glass frit and a laser is promising as a sealing means for an organic EL display.
- a glass frit is formed by heating and melting a powder mixture of components mainly composed of metal oxides to vitrify, and then finely pulverizing the powder to form a paste with a solution in which an organic binder is usually dissolved in an organic solvent. It is applied to the part and remelted by heating to form a sealing glass layer.
- glass frit having various glass compositions not containing toxic lead has been put into practical use, and is widely used as a sealing part for keeping the inside of LCD, PDP, fluorescent display tube (VFD), etc. at a high vacuum.
- the organic EL element that is sensitive to moisture is also suitable for shielding from the outside air.
- the sealing temperature of a general glass frit is 400 ° C. or more
- Patent Documents 1 to 4 is promising.
- such laser sealing has an advantage that the sealing time can be greatly shortened as compared with sealing by heating in the furnace.
- glass frit which has been widely used for sealing flat displays in the past, generally has a bright color tone and is poor in laser light absorption. Therefore, it is necessary to add metal powder such as iron or manganese to increase the absorption. As a result, the material cost is high, and it takes time and effort to prepare the frit, and the insulation is lowered. On the other hand, even when laser sealing is performed, it is desirable that the glass frit softens at a lower temperature in order to reduce the thermal adverse effect on the organic EL element, and it is possible to ensure sealing and increase the sealing strength.
- the thermal expansion coefficient of the glass frit close to the thermal expansion coefficient of the glass substrate. Furthermore, when sealing continuously in mass production of organic EL displays, the glass frit has high stability and crystal precipitation during melting in order to relax the sealing conditions and suppress the occurrence of errors due to fluctuations in the conditions. It is desirable that it does not occur easily. However, the conventional glass frit has not been able to exhibit satisfactory performance in terms of low temperature softening property, thermal expansion coefficient, stability, and the like.
- the present invention can exhibit high absorbability with respect to laser light without adding metal powder as a lead-free glass material for sealing an organic EL, and thus good sealing quality can be obtained by laser sealing.
- it has excellent low temperature softening properties and stability at melting, has a small coefficient of thermal expansion, reduces the amount of heat input at the time of sealing, and sufficiently suppresses the adverse thermal effects of the organic EL element, while strictly sealing conditions.
- the main purpose is to provide a device capable of achieving high sealing performance and high sealing strength with high yield without requiring management control.
- Another object of the present invention is to provide an organic EL display of excellent quality and a method for efficiently and reliably manufacturing the display by using the above-mentioned lead-free glass material for sealing an organic EL.
- the lead-free glass material for sealing an organic EL according to the invention of claim 1 is 30% to 60% V 2 O 5 , 5 to 20% ZnO, 5 to 20% in terms of mol%.
- the lead-free glass material for sealing an organic EL according to the invention of claim 2 is expressed in terms of mol%, 35 to 55% V 2 O 5 , 10 to 18% ZnO, 5 to 18% BaO, 15 to 30 % TeO 2 , 0-7% Nb 2 O 5 , 0-5% Al 2 O 3 , 0-5% SiO 2 , 0-5% MgO, 0-5% Sb 2 O 3 , 0-4% CuO, 0-4% SnO, Nb 2 O 5 + Al 2 O 3 2-8%, SiO 2 + MgO + Sb 2 O 3 0-5%, CuO + SnO 0-4% It is characterized by having a certain glass composition.
- SiO 2 + MgO + Sb 2 O 3 in the glass composition is 0.5 to 5 mol%.
- CuO + SnO in the glass composition is 0.5 to 4 mol%.
- the filler in the lead-free glass material for sealing an organic EL according to any one of the first to fourth aspects, is 50/50 in a weight ratio of glass powder / filler to the glass powder having the glass composition. It is supposed to be blended in the range of ⁇ 99/1.
- the organic EL display according to the invention of claim 6 is formed by sealing between the peripheral portions of the opposing glass substrates with the lead-free glass material for sealing an organic EL described in any one of 1 to 5 above.
- the glass substrate has a thermal expansion coefficient of 35 ⁇ 10 ⁇ 7 / ° C. to 50 ⁇ 10 ⁇ 7 / ° C.
- the method for producing an organic EL display according to the invention of claim 8 comprises interposing the lead-free glass material for sealing an organic EL according to any one of claims 1 to 5 between the peripheral portions of the glass substrates facing the organic EL display.
- the glass material is heated and melted by laser light irradiation to seal between the peripheral portions of both glass substrates.
- a method for producing an organic EL display comprising: preparing a frit paste by adding an organic binder solution to the lead-free glass material powder for sealing an organic EL according to any one of the first to fifth aspects; After the paste is applied to at least one peripheral part of a pair of glass substrates facing the organic EL display and pre-baked at a softening point of + 50 ° C. to + 120 ° C., the organic components of the coating layer are volatilized and removed. By overlapping both glass substrates through this coating layer and irradiating the coating layer with laser light, the glass component of the coating layer is melted to seal between the peripheral portions of both glass substrates. It is characterized by.
- a lead-free glass material for sealing an organic EL four components of V 2 O 5 , ZnO, BaO and TeO 2 and at least one of Nb 2 O 5 and Al 2 O 3 are essential components.
- the glass transition point and the softening point are low, the low-temperature workability is low, the thermal expansion coefficient is small, the fluidity and stability during melting are good, and the absorption of laser light is also good
- laser sealing with a small amount of heat input suppresses thermal shock to the organic EL element and ensures good display performance, while maintaining high yield without requiring strict management control of sealing conditions What can achieve the performance and the high sealing strength is provided.
- the lead-free organic EL sealing comprising the four components V 2 O 5 , ZnO, BaO, and TeO 2 and at least one of Nb 2 O 5 and Al 2 O 3 as essential components.
- each component has a glass composition with a more suitable ratio, so that it is superior in low-temperature workability, and can ensure high sealing quality by reliably avoiding thermal shock to the organic EL element by laser sealing.
- a specific amount of filler is blended with the glass powder of the glass composition, so that the thermal expansion coefficient of the sealing glass layer is organic.
- the sealing property can be improved by reliably approaching the thermal expansion property of the glass substrate of the EL display, and the strength of the sealing glass layer is improved.
- the organic EL display is sealed with the above-mentioned lead-free glass material for sealing the organic EL, the organic EL element inside is completely removed from the outside air. Therefore, it is possible to provide a liquid crystal display device that is excellent in sealing strength of the sealing portion and that can stably exhibit good display performance over a long period of time.
- the lead-free glass material for sealing the organic EL is interposed between the peripheral portions of the glass substrates facing the organic EL display, and the glass material is used for the laser light. Because it is heated and melted by irradiation to seal between the peripheral parts of both glass substrates, the amount of heat input associated with sealing is reduced to suppress thermal shock to the organic EL element, and strict control of sealing conditions Without requiring control, an organic EL display having good sealing quality and excellent durability can be mass-produced with high efficiency and high yield.
- the lead-free glass material for sealing the organic EL is pasted and applied to the peripheral portion of the glass substrate, and pre-baked at a specific temperature to be applied. After stripping and removing the organic components, the two glass substrates are overlapped and laser-sealed through this coating layer, so the amount of heat input during laser sealing is reduced and the thermal adverse effect on the organic EL element is reduced. There is an advantage that it can be further reduced and the assembly operation of the member in the preparation stage of sealing can be easily and reliably performed.
- the lead-free glass material for organic EL sealing according to the present invention is basically composed of V 2 O 5 —ZnO—BaO—TeO 2 in addition to a quaternary glass composition of Nb 2 O 5 and Al 2 O 3 . It contains at least one of the essential components and is superior in low-temperature workability compared to a lead-free glass material having a glass composition comprising four components of V 2 O 5 —ZnO—BaO—TeO 2 , and good flow at a low melting temperature. In addition to exhibiting properties and glass luster, the coefficient of thermal expansion is remarkably small, the color tone is relatively dark, the laser light absorption is high, and the water resistance and chemical resistance are also excellent.
- this lead-free glass material is used for sealing between the glass substrates of the organic EL display, laser sealing can be performed with a small amount of heat input, and the thermal adverse effect on the organic EL element can be reliably suppressed, and the glass substrate and the sealing can be sealed. It was easy to adapt the thermal expansibility with the glass stop layer, so that very excellent sealing properties and large sealing strength could be imparted, and the water resistance and chemical resistance of the sealing glass layer were also improved.
- the organic EL display has excellent durability and can exhibit high display performance over a long period of time.
- the ratio of each component of such an organic EL sealing lead-free glass material is expressed in mol%, V 2 O 5 is 30 to 60%, ZnO is 5 to 20%, BaO is 5 to 20%, and TeO 2 is 15 Nb 2 O 5 is 0 to 7%, Al 2 O 3 is 0 to 7%, and the total amount of Nb 2 O 5 and Al 2 O 3 is 0.5 to 10%.
- the softening point [Tf] is less than 320 ° C.
- the glass transition point [Tg] is less than 300 ° C.
- sealing processing at a low temperature is possible.
- the coefficient of thermal expansion is as small as 110 ⁇ 10 ⁇ 7 / ° C. to 130 ⁇ 10 ⁇ 7 / ° C., and it generally exhibits a dark brown color with good laser light absorption.
- Nb 2 O 5 and Al 2 O 3 greatly improves the low-temperature workability and greatly reduces the coefficient of thermal expansion, and the stability of the glass
- the water resistance and chemical resistance are also increased.
- each exceeds 7 mol% or the total amount exceeds 10 mol% the low temperature workability deteriorates even if the thermal expansion coefficient further decreases.
- the total amount of both is less than 0.5 mol%, a sufficient blending effect cannot be obtained.
- the stability of the glass can be improved by increasing the blending amount of TeO 2 from the specified range. However, in this case, there is a problem that the thermal expansion coefficient is greatly increased.
- a more preferable glass composition is expressed in mol%, V 2 O 5 is 35 to 55%, ZnO is 10 to 18%, BaO is 5 to 18%, TeO 2 is 15 to 30%, Nb 2 O 5 Is 0 to 7%, Al 2 O 3 is 0 to 5%, and the total amount of Nb 2 O 5 and Al 2 O 3 is 2 to 8%.
- the lead-free glass material for sealing an organic EL of the present invention in addition to the above six components of V 2 O 5 , ZnO, BaO, TeO 2 , Nb 2 O 5 , and Al 2 O 3 , if necessary Various other oxide components may be blended. As particularly preferred in such optional ingredients, SiO 2, MgO, Sb 2 O 3, CuO, 5 kinds of SnO, and the like.
- B 2 O 3 that is commonly used as a component of lead-free glass materials for sealing, when added to the above glass composition, increases the glass transition point (Tg) and softening point (Tf) and in a molten state. Therefore, it is desirable not to contain it substantially.
- all of the three components of SiO 2 , MgO, and Sb 2 O 3 have the effect of reducing the thermal expansion coefficient by additionally blending into the glass composition, but the blending amount is If the amount is too large, low-temperature processability is impaired. For this reason, the blending amount of these three kinds is 0 to 5 mol% when used alone, and the total amount (SiO 2 + MgO + Sb 2 O 3 ) is 0 to 5 mol%, but the total amount is 0.1 mol%. If it is less than the range, the blending effect is not recognized. To obtain a substantially sufficient blending effect, the total amount is preferably in the range of 0.5 to 5 mol%.
- two components of CuO and SnO also have the effect of reducing the thermal expansion coefficient by additional blending.
- the fluidity at the time is significantly deteriorated.
- the blending amount of these two types is 0 to 4 mol% when used alone, and 0 to 4 mol% even when the total amount (CuO + SnO) is used, but if the total amount is less than 0.1 mol%, it is substantially blended.
- the total amount is preferably in the range of 0.5 to 4 mol%.
- the raw material powder mixture is put in a container such as a platinum crucible, and this is baked and melted for a predetermined time in a heating furnace such as an electric furnace.
- the melt may be poured into an appropriate formwork such as an alumina boat and cooled, and the obtained glass block may be pulverized to an appropriate particle size by a pulverizer to form a glass frit.
- the particle size of the glass frit is preferably in the range of 0.05 to 100 ⁇ m, and the coarse particles resulting from the pulverization may be classified and removed.
- the particle size is 10 ⁇ m or less, more preferably 6 ⁇ m or less.
- various pulverizers such as jet mills conventionally used for glass frit production can be used.
- wet pulverization is preferably used for a fine particle size of 3 ⁇ m or less.
- This wet pulverization is performed using a media (ball) or bead mill made of alumina or zirconia with a diameter of 5 mm or less in an aqueous solvent such as water or an alcohol aqueous solution, and is pulverized more finely than jet mill pulverization.
- the glass composition as a material to be pulverized needs to have high water resistance, and the glass material of the present invention is also suitable in this respect.
- the lead-free glass material for organic EL sealing of the present invention is a mixture form in which a filler such as a filler or an aggregate is mixed with the glass powder, in addition to using the glass powder (glass frit) having the glass composition alone. It is good.
- a filler reduces the thermal expansion coefficient of the sealing glass layer depending on the blending thereof. Therefore, the thermal expansion of the sealing glass layer can be easily adjusted to the thermal expansion of the glass substrate of the organic EL display by adjusting the blending amount. Can be adapted.
- the glass component functions as a binder that binds the filler particles to each other at the time of heating and melting, so that the obtained sealing glass layer becomes a sintered body having a high strength and a dense ceramic form.
- the filler is not particularly limited as long as it has a higher melting point than the glass component and does not melt at the firing temperature during processing.
- zirconium silicate, cordierite, zirconium phosphate, ⁇ ⁇ eucryptate , ⁇ -spodumene, zircon, alumina, mullite, silica, ⁇ -quartz solid solution, zinc silicate, aluminum titanate and the like are suitable. Therefore, the blending amount of these fillers is preferably in the range of 50/50 to 99/1 as a weight ratio of glass powder / filler. If the amount is too large, the fluidity at the time of melting deteriorates and the binding force by the glass composition is insufficient, so that a strong sintered body cannot be formed.
- the thermal expansion coefficient of the glass substrate used for the organic EL display is generally about 35 ⁇ 10 ⁇ 7 / ° C. to 50 ⁇ 10 ⁇ 7 / ° C.
- the thermal expansion coefficient of the glass powder itself is low, sealing is performed while ensuring sufficient fluidity in a molten state by adjustment by blending of fillers.
- the thermal expansion coefficient of the glass layer can be reduced to about 50 ⁇ 10 ⁇ 7 / ° C.
- the lead-free glass material having the glass composition composed of the four components V 2 O 5 —ZnO—BaO—TeO 2 described above fluidity in the molten state is ensured even if adjustment is made by blending the filler.
- the thermal expansion coefficient of the sealing glass layer can be reduced only to about 60 ⁇ 10 ⁇ 7 / ° C.
- the glass powder (glass frit) of the lead-free glass material for sealing an organic EL of the present invention and the mixed powder obtained by mixing the filler with the glass powder are generally used as a paste having a high concentration dispersed in an organic binder solution. Since it is applied to the peripheral part of at least one glass substrate to be disposed opposite to the organic EL display panel by screen printing or the like and subjected to firing, it may be commercialized as a paste form in advance.
- the organic binder solution used for the paste is not particularly limited, but for example, cellulose binders such as nitrocellulose and ethyl cellulose, butyl carbitol acetate, butyl diglycol acetate, terpineol, pine oil, aromatic hydrocarbon solvents.
- cellulose binders such as nitrocellulose and ethyl cellulose, butyl carbitol acetate, butyl diglycol acetate, terpineol, pine oil, aromatic hydrocarbon solvents.
- a solvent such as a mixed solvent such as thinner
- the viscosity of the paste is preferably in the range of 30 to 3000 dPa ⁇ s from the viewpoint of coating workability.
- the glass material is interposed between the peripheral portions of the opposing glass substrates of the organic EL display panel, and the glass materials are heated and melted to form both glass substrates. Seal between the peripheries. At this time, it is not impossible for the glass material to be interposed between both glass substrates in the form of a powder or a thin plate, but at least one glass substrate (usually as the paste) is used to form an extremely thin sealing glass layer. A method of applying to the sealing glass plate side where the organic EL element is not applied is recommended. The glass material can be heated and melted by holding it in a high-temperature atmosphere in a heating furnace.
- the organic EL element in order to avoid thermal deterioration of the organic EL element, as described above, it is locally applied by laser light irradiation. It is good to carry out by manual heating. Since the glass powder exhibits a dark brown color with good laser light absorption as described above, laser sealing can be applied without any trouble even if a conventional metal powder is not included.
- the heat treatment for the sealing process can be performed once, but it is preferable to perform it in two stages in order to improve the sealing quality. That is, by first heating to near the softening point [Tf] of the glass material as temporary firing, the vehicle components (binder and solvent) of the paste are volatilized and pyrolyzed to leave only the frit component, and then laser firing as the main firing. A sealed glass layer in which the glass components are completely melted and integrated is formed by local heating by light irradiation.
- the vehicle component is volatilized and removed in the first stage of preliminary firing, and the glass components are fused together in the second stage of final firing. And pinholes due to deaeration can be prevented, and the reliability of sealing and the strength of the sealing portion can be increased.
- organic EL elements that are subject to thermal degradation are placed inside, and the electrodes before the assembly are fixed by sandwiching electrodes, lead wires, exhaust pipes, etc. After the first stage heat treatment is performed only on the coated glass substrate, it is assembled into a product form using this glass substrate and other required members, and the second stage heat treatment is performed in this assembled state to produce an organic EL element. The thermal adverse effects of can be further reduced.
- the organic EL display panel of the present invention is composed of a sealing glass layer using the above-described lead-free glass material for sealing an organic EL of the present invention in the schematic configuration shown in FIG.
- the sealing layer 6 has a high hermetic holding force as a melted and solidified product of glass frit, and has adhesion and adhesion strength to the surfaces of both glass substrates opposed to each other, that is, the EL element substrate 1 and the sealing glass plate 5. In addition to providing excellent sealing properties and high sealing strength, it exhibits good water resistance and chemical resistance.
- the durability of the sealing portion is excellent, good display performance can be stably exhibited over a long period of time, and it is not necessary to dispose a water capturing agent or a desiccant inside the package. Since the panel configuration is simple, assembly and manufacture can be done easily at low cost, and water is difficult to adsorb to the glass material with excellent water resistance, so water vapor is generated as outgas from the glass frit during sealing processing. There is no concern that the water vapor enters the package and degrades the organic EL element.
- the results are shown in Tables 1 to 3 below.
- the measurement method for each item is as follows.
- Glass transition point, softening point, crystallization start temperature Using a differential thermal analyzer (TG-8120 manufactured by Rigaku Corporation), ⁇ -alumina was used as a reference (standard sample), and the sample glass was measured at a heating rate of 10 ° C./min and a temperature range of 25 ° C. (room temperature) to 600 ° C. A transition point [Tg], a softening point [Tf], and a crystallization start temperature [Tx] were measured.
- thermomechanical analyzer TMA8310 manufactured by Rigaku Corporation.
- the lead-free glass material powder is melted again, and this is formed into a square column of 5 ⁇ 5 ⁇ 20 mm (length ⁇ width ⁇ height), and the upper bottom surface is formed in parallel and used as a measurement sample.
- the temperature was raised from room temperature to 250 ° C. at a rate of 10 ° C./min, and the average thermal expansion coefficient ⁇ was determined.
- quartz glass was used for the standard sample.
- the basic composition is composed of four components of V 2 O 5 , ZnO, BaO and TeO 2 at appropriate ratios, and one or both of Nb 2 O 5 and Al 2 O 3 are in the appropriate range.
- the lead-free glass material (No. 2, 4, 6-8, 10) of the present invention having a glass composition added in addition has a glass transition point [Tg] of 275-295 ° C. and a softening point [Tf] of 285-316.
- Lead-free glass material consisting of the above four components of the above-mentioned basic composition, which has a low fluidity and glass luster at a low temperature of less than 420 ° C. and exhibits good fluidity and glass luster and also has a low thermal expansion coefficient.
- the glass transition point [Tg] is 285 ° C. or less, the softening point.
- [Tf] is also very low at 298 ° C. or less, and it can be seen that it has extremely excellent low-temperature workability.
- lead-free glass materials No. 2, 4, 6, 8, 10
- Lead-free glass materials (No. 26 to No. 26 to 4) of V 2 O 5 , ZnO, BaO, TeO 2 and 5 components obtained by adding Nb 2 O 5 to these 4 components and B 2 O 3 additionally added In 29), the thermal expansion coefficient is reduced as compared with the lead-free glass material (No. 1) composed of the four components, but the low-temperature workability is not improved, and the glass is devitrified and is good. There is a drawback that the heating temperature for obtaining fluidity and glass gloss is increased.
- Production Example 2 The lead-free glass materials No. 1 (Comparative Example) and No. 12 (Example) in Production Example 1 were each zirconia-based filler (zirconium phosphate, maximum particle size of 5.5 ⁇ m, average particle size of about 1. 0 ⁇ m) was mixed at the ratios shown in Table 2 below to produce lead-free glass materials No. 30 and No. 31 containing a refractory filler. And about these lead-free glass materials No.30 and 31, the thermal expansion coefficient, the fluidity
- a frit paste was prepared by adding and mixing 20 g of a vehicle made of ethyl cellulose / butyl carbitol acetate / terpineol to 100 g of each of lead-free glass materials No. 30 and 31 containing a refractory filler obtained in Production Example 2 to prepare a frit paste.
- a non-alkali glass substrate (length: 40 mm, width: 30 mm, thickness: 0.7 mm, thermal expansion coefficient: 40 ⁇ 10 ⁇ 7 / ° C.) is coated with the frit paste at a line width of 0.6 mm and a thickness of about 10 ⁇ m. It applied so that the rectangle of * 20mm might be drawn.
- the non-alkali glass substrate of the same dimension is overlapped on the frit coated surface side of the glass substrate in a state of being displaced in the longitudinal direction and clipped.
- the glass component of the frit is irradiated by irradiating a laser beam of a semiconductor laser (wavelength 808 nm) at an irradiation speed of 2 mm / sec along the frit paste coating line with the glass substrate on the pre-fired side as the upper surface. It was melted and sealed.
- This pair of sealed glass substrates is fixed vertically, and a pressure is applied downward at 1000 N / min or lower to the upper end of the upper glass substrate due to the above-mentioned positional deviation, and the peak pressure when the sealing surface peels off.
- the sealing force per unit area was calculated from the results shown in Table 4.
- the lead-free glass material No. 31 containing a refractory filler that is an example of the present invention has a coefficient of thermal expansion that is higher than that of the lead-free glass material No. 30 containing a refractory filler that is a comparative example.
- the coefficient of thermal expansion of the glass substrate is very close, so that a high sealing property is obtained, the sealing strength is nearly doubled, and good fluidity and glass gloss are exhibited at a lower temperature. Therefore, it can be seen that it is excellent in low-temperature workability.
- lead-free glass material No. 31 containing a refractory filler as an example of the present invention is superior in water resistance and acid resistance compared to lead-free glass material No. 30 containing a refractory filler in a comparative example.
- the alkali resistance is not inferior, and it is clear that excellent durability can be imparted to the organic EL display by using it as a sealing material.
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Abstract
Description
原料酸化物としてV2O5、ZnO、BaO、TeO2、Nb2O5、Al2O3、SiO2、MgO、Sb2O3、CuO、SnO、B2O3の各粉末を後記表1~3に記載の比率(モル%)で混合したもの(全量10g)を白金るつぼに収容し、電気炉内で約1000℃にて60分間加熱して溶融させたのち、その溶融物をアルミナポートに流し込んでガラスバーを作成し、大気中で冷却後に該ガラスバーを自動乳鉢にて粉砕し、この粉砕物を分級して粒径100μm以下のものを採取し、粉末状の無鉛ガラス材No.1~29を製造した。
示差熱分析装置(リガク社製TG-8120)により、リファレンス(標準サンプル)としてα-アルミナを用い、加熱速度10℃/分、温度範囲25℃(室温)~600℃の測定条件でサンプルのガラス転移点〔Tg〕、軟化点〔Tf〕、結晶化開始温度〔Tx〕を測定した。
熱機械分析装置(リガク社製TMA8310)により、熱膨張係数を測定した。この測定は、無鉛ガラス材粉末を再度溶融し、これを5×5×20mm(縦×横×高さ)の四角柱に成形し、上底面が平行に成形されたものを測定試料として用い、常温~250℃まで10℃/分で昇温させ、平均熱膨張係数αを求めた。また、標準サンプルには石英ガラスを用いた。
各無鉛ガラス材を型内で溶融・硬化させて径8.8mm、厚さ2.0mmのボタン状の成形試料を作製し、この成形試料をガラス基板上に載置した状態で、電気炉内で加熱速度10℃/分で加熱して昇温させてゆき、420℃、450℃、500℃の各温度で10分間保持後に室温まで冷却し、成形試料の状態変化を観察し、次の4段階で評価した。
◎・・・420℃未満で良好な流動性及びガラス光沢を示す。
○・・・420℃以上~450℃未満で良好な流動性及びガラス光沢を示す。
△・・・450℃以上~500℃未満で良好な流動性及びガラス光沢を示す。
×・・・500℃未満では良好な流動性及びガラス光沢を示さない。
前記製造例1における無鉛ガラス材No.1(比較例)及びNo.12(実施例)の粉末に対し、それぞれジルコニア系フィラー(リン酸ジルコニウム、最大粒子径5.5μm、平均粒子径約1.0μm)を後記表2に記載の比率で混合し、耐火物フィラー入り無鉛ガラス材No.30及びNo.31を製造した。そして、これら無鉛ガラス材No.30,31について、熱膨張係数と溶融状態での流動性及びガラス光沢を前記同様にして調べ、これらの結果を次の封着試験による封着強度の測定値と共に表4に示す。なお、流動性及びガラス光沢は製造例1と同様の4段階評価とした。
前記製造例2で得られた耐火物フィラー入り無鉛ガラス材No.30,31の各100gに対し、エチルセルロース/ブチルカルビトールアセテート/ターピネオールからなるビークル20gを添加混合してフリットペーストを調製し、矩形の無アルカリガラス基板(長さ40mm、幅30mm、厚さ0.7mm、熱膨張係数40×10-7/℃)の片面に、該フリットペーストを線幅0.6mm、厚さ約10μmで30×20mmの矩形を描くように塗着した。そして、このガラス基板を電気炉中で300℃にて60分間仮焼成したのち、該ガラス基板のフリット塗着面側に同寸法の無アルカリガラス基板を長手方向に位置ずれした状態に重ねてクリップで固定し、その仮焼成側のガラス基板を上面として前記フリットペーストの塗着ラインに沿い、半導体レーザー(波長808nm)のレーザー光を照射速度2mm/秒で照射することにより、フリットのガラス成分を溶融させて封着を行った。この封着した一対のガラス基板を垂直に固定し、上記位置ずれで上位になったガラス基板の上端に1000N/分以下で下向きに圧力を加えてゆき、封着面が剥離したときのピーク圧から単位面積当たりの封着力(圧縮剪断強度)を算出し、封着強度として表4に示す。
前記製造例2で得られた耐火物フィラー入り無鉛ガラス材No.30,31について、型内で溶融・硬化させて約1gの角柱状試料(長さ約6.3mm)を作製し、この角柱状試料を各々500mLの水、1モル濃度のHCl水、1モル濃度のNaOH水が入った容器の液中に浸漬し、この各容器を70℃の恒温槽に収容し、所定時間毎に試料を取り出して100℃,1時間の乾燥を行い、自然冷却後の試料の重量を測定し、初期重量からの重量減少率を次式で算出した。その結果を表5に示す。
重量減少率(%)=〔1-測定重量(g)/初期重量(g)〕×100
2 下部電極
3 有機発光層
4 上部電極
5 封止ガラス板(ガラス基板)
6 シール層(封着ガラス層)
Claims (9)
- モル%表示で、30~60%のV2O5、5~20%のZnO、5~20%のBaO、15~40%のTeO2、0~7%のNb2O5、0~7%のAl2O3、0~5%のSiO2、0~5%のMgO、0~5%のSb2O3、0~4%のCuO、0~4%のSnOを含み、且つNb2O5+Al2O3が0.5~10%、SiO2+MgO+Sb2O3が0~5%、CuO+SnOが0~4%であるガラス組成を有してなる有機EL封着用無鉛ガラス材。
- モル%表示で、35~50%のV2O5、10~18%のZnO、5~18%のBaO、15~30%のTeO2、0~7%のNb2O5、0~5%のAl2O3、0~5%のSiO2、0~5%のMgO、0~5%のSb2O3、0~4%のCuO、0~4%のSnOを含み、且つNb2O5+Al2O3が2~8%、SiO2+MgO+Sb2O3が0~5%、CuO+SnOが0~4%であるガラス組成を有してなる有機EL封着用無鉛ガラス材。
- 前記ガラス組成におけるSiO2+MgO+Sb2O3が0.5~5モル%である請求項1又は2に記載の有機EL封着用無鉛ガラス材。
- 前記ガラス組成におけるCuO+SnOが0.5~4モル%である請求項1~3のいずれかに記載の有機EL封着用無鉛ガラス材。
- 前記ガラス組成を有するガラス粉末に対してフィラーが、ガラス粉末/フィラーの重量比で50/50~99/1の範囲で配合されてなる請求項1~4の何れかに記載の有機EL封着用無鉛ガラス材。
- 請求項1~5のいずれかに記載の有機EL封着用無鉛ガラス材により、対向するガラス基板の周辺部間が封着されてなる有機ELディスプレイ。
- 前記ガラス基板の熱膨張係数が35×10-7/℃~50×10-7/℃である請求項6記載の有機ELディスプレイ。
- 有機ELディスプレイの対向するガラス基板の周辺部間に前記請求項1~5のいずれかに記載の有機EL封着用無鉛ガラス材を介在させ、このガラス材をレーザー光の照射によって加熱溶融させて両ガラス基板の周辺部間を封着することを特徴とする有機ELディスプレイの製造方法。
- 前記請求項1~5のいずれかに記載の有機EL封着用無鉛ガラス材の粉末に有機バインダー溶液を加えてフリットペーストを調製し、このフリットペーストを有機ELディスプレイの対向配置させる一対のガラス基板の少なくとも一方の周辺部に塗着して軟化点+50℃~+120℃で仮焼成することにより、塗着層の有機成分を揮散除去したのち、この塗着層を介して両ガラス基板を重ね合わせて該塗着層にレーザー光を照射することにより、該塗着層のガラス成分を溶融させて両ガラス基板の周辺部間を封着することを特徴とする有機ELディスプレイの製造方法。
Priority Applications (6)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
EP10847017.0A EP2525626B1 (en) | 2010-03-05 | 2010-03-05 | Lead-free glass material for organic-el sealing, organic el display formed using the same |
JP2012502950A JP5713993B2 (ja) | 2010-03-05 | 2010-03-05 | 有機el封着用無鉛ガラス材とこれを用いた有機elディスプレイ及び該ディスプレイの製造方法 |
PCT/JP2010/053670 WO2011108115A1 (ja) | 2010-03-05 | 2010-03-05 | 有機el封着用無鉛ガラス材とこれを用いた有機elディスプレイ及び該ディスプレイの製造方法 |
KR1020127019459A KR101626840B1 (ko) | 2010-03-05 | 2010-03-05 | 유기 el 봉착용 무연 유리재와 이것을 사용한 유기 el 디스플레이 |
CN201080064524.7A CN102918927B (zh) | 2010-03-05 | 2010-03-05 | 有机el封装用无铅玻璃材料和使用它的有机el显示器 |
US13/593,165 US8766524B2 (en) | 2010-03-05 | 2012-08-23 | Lead-free glass material for organic-EL sealing, organic EL display formed using the same |
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PCT/JP2010/053670 WO2011108115A1 (ja) | 2010-03-05 | 2010-03-05 | 有機el封着用無鉛ガラス材とこれを用いた有機elディスプレイ及び該ディスプレイの製造方法 |
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US13/593,165 Continuation US8766524B2 (en) | 2010-03-05 | 2012-08-23 | Lead-free glass material for organic-EL sealing, organic EL display formed using the same |
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WO2011108115A1 true WO2011108115A1 (ja) | 2011-09-09 |
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US (1) | US8766524B2 (ja) |
EP (1) | EP2525626B1 (ja) |
JP (1) | JP5713993B2 (ja) |
KR (1) | KR101626840B1 (ja) |
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KR20130025362A (ko) | 2013-03-11 |
US20120321902A1 (en) | 2012-12-20 |
KR101626840B1 (ko) | 2016-06-02 |
CN102918927B (zh) | 2015-08-19 |
EP2525626A4 (en) | 2014-11-12 |
EP2525626B1 (en) | 2018-05-02 |
JP5713993B2 (ja) | 2015-05-07 |
EP2525626A1 (en) | 2012-11-21 |
JPWO2011108115A1 (ja) | 2013-06-20 |
US8766524B2 (en) | 2014-07-01 |
CN102918927A (zh) | 2013-02-06 |
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