KR20130134564A - Frit composition for sealing electric component panels and electric components sealed with said frit composition - Google Patents
Frit composition for sealing electric component panels and electric components sealed with said frit composition Download PDFInfo
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- KR20130134564A KR20130134564A KR1020120058166A KR20120058166A KR20130134564A KR 20130134564 A KR20130134564 A KR 20130134564A KR 1020120058166 A KR1020120058166 A KR 1020120058166A KR 20120058166 A KR20120058166 A KR 20120058166A KR 20130134564 A KR20130134564 A KR 20130134564A
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- 239000000203 mixture Substances 0.000 title claims abstract description 64
- 238000007789 sealing Methods 0.000 title claims abstract description 56
- 239000011521 glass Substances 0.000 claims abstract description 23
- 238000000034 method Methods 0.000 claims description 19
- 239000000945 filler Substances 0.000 claims description 15
- 150000002500 ions Chemical class 0.000 claims description 15
- 229910001456 vanadium ion Inorganic materials 0.000 claims description 15
- 238000002360 preparation method Methods 0.000 claims description 6
- 239000003638 chemical reducing agent Substances 0.000 claims description 5
- 239000008393 encapsulating agent Substances 0.000 claims description 5
- 229910010413 TiO 2 Inorganic materials 0.000 claims description 4
- 229910015902 Bi 2 O 3 Inorganic materials 0.000 claims description 3
- 239000012298 atmosphere Substances 0.000 claims description 3
- 150000003682 vanadium compounds Chemical class 0.000 claims description 3
- 229910052802 copper Inorganic materials 0.000 claims description 2
- 229910052718 tin Inorganic materials 0.000 claims description 2
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 claims 1
- 229910052698 phosphorus Inorganic materials 0.000 claims 1
- 239000011574 phosphorus Substances 0.000 claims 1
- 230000006866 deterioration Effects 0.000 abstract 1
- 239000000565 sealant Substances 0.000 abstract 1
- 229910052720 vanadium Inorganic materials 0.000 abstract 1
- LEONUFNNVUYDNQ-UHFFFAOYSA-N vanadium atom Chemical compound [V] LEONUFNNVUYDNQ-UHFFFAOYSA-N 0.000 abstract 1
- 239000000758 substrate Substances 0.000 description 22
- 239000003566 sealing material Substances 0.000 description 9
- 239000003792 electrolyte Substances 0.000 description 8
- 229920005989 resin Polymers 0.000 description 7
- 239000011347 resin Substances 0.000 description 7
- 239000000853 adhesive Substances 0.000 description 6
- 230000001070 adhesive effect Effects 0.000 description 6
- WMWLMWRWZQELOS-UHFFFAOYSA-N bismuth(iii) oxide Chemical compound O=[Bi]O[Bi]=O WMWLMWRWZQELOS-UHFFFAOYSA-N 0.000 description 6
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 5
- 238000004519 manufacturing process Methods 0.000 description 5
- 230000003287 optical effect Effects 0.000 description 5
- 229910052760 oxygen Inorganic materials 0.000 description 5
- 239000001301 oxygen Substances 0.000 description 5
- 238000005245 sintering Methods 0.000 description 5
- 238000010521 absorption reaction Methods 0.000 description 4
- 238000005538 encapsulation Methods 0.000 description 4
- 238000010304 firing Methods 0.000 description 4
- 238000010438 heat treatment Methods 0.000 description 4
- 238000002156 mixing Methods 0.000 description 4
- 239000004065 semiconductor Substances 0.000 description 4
- 239000002904 solvent Substances 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 3
- 229910052878 cordierite Inorganic materials 0.000 description 3
- JSKIRARMQDRGJZ-UHFFFAOYSA-N dimagnesium dioxido-bis[(1-oxido-3-oxo-2,4,6,8,9-pentaoxa-1,3-disila-5,7-dialuminabicyclo[3.3.1]nonan-7-yl)oxy]silane Chemical compound [Mg++].[Mg++].[O-][Si]([O-])(O[Al]1O[Al]2O[Si](=O)O[Si]([O-])(O1)O2)O[Al]1O[Al]2O[Si](=O)O[Si]([O-])(O1)O2 JSKIRARMQDRGJZ-UHFFFAOYSA-N 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 239000011368 organic material Substances 0.000 description 3
- 230000035515 penetration Effects 0.000 description 3
- 239000002952 polymeric resin Substances 0.000 description 3
- 229910052710 silicon Inorganic materials 0.000 description 3
- 239000010703 silicon Substances 0.000 description 3
- 229920003002 synthetic resin Polymers 0.000 description 3
- 238000002076 thermal analysis method Methods 0.000 description 3
- 229910000166 zirconium phosphate Inorganic materials 0.000 description 3
- LEHFSLREWWMLPU-UHFFFAOYSA-B zirconium(4+);tetraphosphate Chemical compound [Zr+4].[Zr+4].[Zr+4].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O LEHFSLREWWMLPU-UHFFFAOYSA-B 0.000 description 3
- RWWJXIAEEFWUSU-UHFFFAOYSA-K P(=O)([O-])([O-])[O-].[W+4].[Zr+4] Chemical compound P(=O)([O-])([O-])[O-].[W+4].[Zr+4] RWWJXIAEEFWUSU-UHFFFAOYSA-K 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 2
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 2
- 229910021417 amorphous silicon Inorganic materials 0.000 description 2
- 239000006121 base glass Substances 0.000 description 2
- 239000011230 binding agent Substances 0.000 description 2
- 150000001768 cations Chemical class 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 230000001678 irradiating effect Effects 0.000 description 2
- 229910021421 monocrystalline silicon Inorganic materials 0.000 description 2
- 239000005416 organic matter Substances 0.000 description 2
- 229910021420 polycrystalline silicon Inorganic materials 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- OAYXUHPQHDHDDZ-UHFFFAOYSA-N 2-(2-butoxyethoxy)ethanol Chemical compound CCCCOCCOCCO OAYXUHPQHDHDDZ-UHFFFAOYSA-N 0.000 description 1
- VXQBJTKSVGFQOL-UHFFFAOYSA-N 2-(2-butoxyethoxy)ethyl acetate Chemical compound CCCCOCCOCCOC(C)=O VXQBJTKSVGFQOL-UHFFFAOYSA-N 0.000 description 1
- 229920000178 Acrylic resin Polymers 0.000 description 1
- 239000004925 Acrylic resin Substances 0.000 description 1
- 229910018072 Al 2 O 3 Inorganic materials 0.000 description 1
- 229910000505 Al2TiO5 Inorganic materials 0.000 description 1
- 241000220259 Raphanus Species 0.000 description 1
- 239000004110 Zinc silicate Substances 0.000 description 1
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 229910000287 alkaline earth metal oxide Inorganic materials 0.000 description 1
- WUOACPNHFRMFPN-UHFFFAOYSA-N alpha-terpineol Chemical compound CC1=CCC(C(C)(C)O)CC1 WUOACPNHFRMFPN-UHFFFAOYSA-N 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- GHPGOEFPKIHBNM-UHFFFAOYSA-N antimony(3+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Sb+3].[Sb+3] GHPGOEFPKIHBNM-UHFFFAOYSA-N 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- SQIFACVGCPWBQZ-UHFFFAOYSA-N delta-terpineol Natural products CC(C)(O)C1CCC(=C)CC1 SQIFACVGCPWBQZ-UHFFFAOYSA-N 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000005496 eutectics Effects 0.000 description 1
- 239000005357 flat glass Substances 0.000 description 1
- 239000002803 fossil fuel Substances 0.000 description 1
- 230000009477 glass transition Effects 0.000 description 1
- 230000008595 infiltration Effects 0.000 description 1
- 238000001764 infiltration Methods 0.000 description 1
- 229910003471 inorganic composite material Inorganic materials 0.000 description 1
- 229910010272 inorganic material Inorganic materials 0.000 description 1
- 239000011147 inorganic material Substances 0.000 description 1
- 238000004898 kneading Methods 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 125000005641 methacryl group Chemical group 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 239000006060 molten glass Substances 0.000 description 1
- 150000002894 organic compounds Chemical class 0.000 description 1
- 239000006132 parent glass Substances 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000000016 photochemical curing Methods 0.000 description 1
- 230000029553 photosynthesis Effects 0.000 description 1
- 238000010672 photosynthesis Methods 0.000 description 1
- 229920000058 polyacrylate Polymers 0.000 description 1
- 229920006254 polymer film Polymers 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- AABBHSMFGKYLKE-SNAWJCMRSA-N propan-2-yl (e)-but-2-enoate Chemical compound C\C=C\C(=O)OC(C)C AABBHSMFGKYLKE-SNAWJCMRSA-N 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000011342 resin composition Substances 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- HUAUNKAZQWMVFY-UHFFFAOYSA-M sodium;oxocalcium;hydroxide Chemical compound [OH-].[Na+].[Ca]=O HUAUNKAZQWMVFY-UHFFFAOYSA-M 0.000 description 1
- 229940116411 terpineol Drugs 0.000 description 1
- 229920001169 thermoplastic Polymers 0.000 description 1
- 229920001187 thermosetting polymer Polymers 0.000 description 1
- 239000004416 thermosoftening plastic Substances 0.000 description 1
- RBNWAMSGVWEHFP-UHFFFAOYSA-N trans-p-Menthane-1,8-diol Chemical compound CC(C)(O)C1CCC(C)(O)CC1 RBNWAMSGVWEHFP-UHFFFAOYSA-N 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
- 238000007740 vapor deposition Methods 0.000 description 1
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 description 1
- 229920002554 vinyl polymer Polymers 0.000 description 1
- XSMMCTCMFDWXIX-UHFFFAOYSA-N zinc silicate Chemical compound [Zn+2].[O-][Si]([O-])=O XSMMCTCMFDWXIX-UHFFFAOYSA-N 0.000 description 1
- 235000019352 zinc silicate Nutrition 0.000 description 1
- 229910052726 zirconium Inorganic materials 0.000 description 1
Images
Classifications
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- 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
- C03C8/08—Frit compositions, i.e. in a powdered or comminuted form containing phosphorus
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L31/00—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
- H01L31/04—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof adapted as photovoltaic [PV] conversion devices
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L31/00—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
- H01L31/18—Processes or apparatus specially adapted for the manufacture or treatment of these devices or of parts thereof
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E10/00—Energy generation through renewable energy sources
- Y02E10/50—Photovoltaic [PV] energy
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E10/00—Energy generation through renewable energy sources
- Y02E10/50—Photovoltaic [PV] energy
- Y02E10/542—Dye sensitized solar cells
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- Engineering & Computer Science (AREA)
- Power Engineering (AREA)
- General Physics & Mathematics (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- Electromagnetism (AREA)
- Chemical & Material Sciences (AREA)
- Computer Hardware Design (AREA)
- Physics & Mathematics (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Life Sciences & Earth Sciences (AREA)
- Manufacturing & Machinery (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Geochemistry & Mineralogy (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Glass Compositions (AREA)
Abstract
Description
The present invention relates to a frit composition for sealing an electrical device panel and an electrical device encapsulated with the frit composition, and more particularly, used as an encapsulant for an electrical device panel, wherein 0.01 to 50 mol% of tetravalent vanadium ions ( V 4+ ), frit for encapsulating an electrical device panel comprising 60 to 95% by weight of the base glass and 5 to 40% by weight of the filler having a coefficient of thermal expansion ranging from 65 × 10 −7 / ° C. to 95 × 10 −7 / ° C. It relates to a composition and an electric element sealed with the frit composition.
In general, the electric element was made of an inorganic material including a metal oxide. However, in recent years, organic-inorganic composite materials are attracting attention as a material of such electric devices. In particular, organic materials have been applied to Dye-Sensitized Solar Cells (DSSC) as organic light-emitting device (OLED) 0 and solar cells, which are attracting attention as next generation displays. Used inside the panel in the form of a cell.
Unlike LCDs that require backlight units (BLUs), OLEDs emit their own light and consume less power and are currently being applied to small displays. In particular, OLEDs have been studied quite actively lately because of their wide field of use and their potential for use in electroluminescent devices. For example, OLEDs can be manufactured with a thinner thickness than conventional display panels, are easy to manufacture in manufacturing panels, and are being spotlighted as next-generation displays due to their suitability for flexible displays, which are next-generation displays. In addition, OLED displays are very bright, have excellent color contrast and wide viewing angle, and have many advantages such as high brightness, light weight, low driving voltage. However, OLED displays tend to deteriorate due to the action of oxygen and moisture leaking into the inside and the electrodes of the device, which causes dark spots, pixel shrinkage, etc., and thus the yield decreases. Have In order to solve this problem, various kinds of sealing technologies such as photocuring, thermosetting resin compositions, and sealing techniques by vapor deposition have been developed. However, in order to protect the OLED device, and to secure stability and lifespan, its characteristics are not yet excellent enough.
In addition, as one of the renewable energy to replace the fossil fuel, solar energy is attracting attention. Solar cells using solar energy are largely classified into silicon solar cells and organic compound semiconductor solar cells according to the type of material. Currently commercialized and sold solar cells include monocrystalline and polycrystalline silicon solar cells and amorphous silicon solar cells. Currently, the energy efficiency of monocrystalline silicon solar cells is 18%, the energy efficiency of polycrystalline silicon solar cells is 15%, and the energy efficiency of amorphous silicon solar cells is known to be 10%. Such silicon solar cells utilize a photoelectric conversion principle by applying a semiconductor material. On the other hand, there is a dye-sensitized solar cell as a solar cell using a photoelectrochemical conversion mechanism using the principle of photosynthesis. Dye-sensitized solar cells have a higher theoretical marginal conversion efficiency than conventional silicon solar cells, and thus are expected to further increase efficiency and attract a lot of attention due to their wide application.
When sunlight is absorbed by dye-sensitized solar cells, electron transitions occur in the dye molecules, which are injected into the conduction band of the semiconductor oxide. The injected electrons move to the conductive film through the interparticle interface of the oxide electrode, and the holes generated in the dye molecules are reduced by the electrolyte sealed by the sealing material between both substrates, thereby generating a current.
Conventionally, a polymer resin-based surin polymer film was used to seal the panel of such an OLED or dye-sensitized solar cell. The reason why such a polymer resin is used for panel sealing is that glass frit, which is a general sealing material, has to go through a sintering process because the organic matter inside the panel is damaged because the sintering is performed at a high temperature. Well, the sealing using the polymer resin has a problem such as penetration of moisture and oxygen or leakage of electrolyte, there is a problem that the efficiency of the electrical device is lowered and the durability is weak. Therefore, in order to secure stable driving and lifespan of the dye-sensitized solar cell, a seal is required to prevent moisture or oxygen penetration and excellent chemical resistance to the electrolyte. This demand has been attempted for a sealing method that enables local heating such as low temperature sealing or laser among ceramic-based glass frits used in panel sealing of flat panel displays. Republic of Korea Patent No. 833474 consists of 20 to 80% by weight Bi2O3, 10 to 30% P2O5, 5 to 20% ZnO, 1 to 15% B2O3, 1 to 20% Sb2O3, and 1 to 20% alkaline earth metal oxide, A low melting glass composition for sealing OLED is disclosed, having a Tg (glass transition temperature) of 450 ° C. or lower and a thermal expansion coefficient of 70 to 90 ° 10 −7 / ° C. In addition, the patent publication of the Republic of Korea Patent No. 1084206, the first substrate and the second substrate configured to face each other, the first electrode portion and the second electrode portion disposed on the inner surface facing the first substrate and the second substrate, respectively; It is disposed along the edge between the first substrate and the second substrate to seal the electrolyte and the electrolyte filled between the first substrate and the second substrate, the inner surface of the first substrate of the second substrate A sealing material comprising a first sealing layer and a second sealing layer, each of which is in contact with an inner surface, wherein the first electrode part includes a semiconductor oxide layer on which dye molecules are adsorbed, and the first sealing layer is a thermoplastic glass frit. ), And the second sealing layer is disclosed a dye-sensitized solar cell comprising an organic resin. In addition, the Republic of Korea Patent Publication No. 10-2009-0100649 is composed of a first electrode made of a transparent plate having a porous membrane containing a dye on one side and a second electrode disposed opposite to the first electrode and between the electrodes In the method of manufacturing a dye-sensitized solar cell comprising an electrolyte, 0 to 30 mol% P2O5 on the bonding surface between the first electrode and the second electrode; V 2 O 5 0-50 mol%; ZnO 0-20 mol%; BaO 0-15 mol%; As 2 O 3 0-20 mol%; Sb 2 O 3 0-20 mol%; In 2 O 3 0-5 mol%; Fe 2 O 3 0-10 mol%; Al 2 O 3 0-5 mol%; B 2 O 3 0-20 mol%; Bi2O3 0-10 mol%; And coating a glass frit containing 0 to 10 mol% of TiO 2, and firing the glass frit to seal the first electrode and the second electrode at a predetermined interval and sealing the same. Is disclosed.
However, the glass frit composition applied in the prior art including the above literature uses a laser encapsulation method or undergoes a sintering process. In the case of sintering, even if it is a low temperature baking, the organic substance inside the panel may be thermally damaged, which is not preferable. Even in the case of sealing using a laser, the glass frit is not irradiated directly with the laser but is irradiated with a resin encapsulant, so that a conventional problem cannot be completely solved. This will cause bigger problems.
Therefore, the technical problem to be achieved by the present invention is effective in preventing moisture or oxygen infiltration without containing lead and having excellent chemical resistance to electrolytes and high absorption rate against electromagnetic waves in the wavelength range of 200 nm to 10,000 nm, which is suitable for laser encapsulation. It is to provide a frit composition for sealing an electrical device panel.
In order to achieve the above technical problem, the present invention is used as an encapsulant of an electrical device panel, and includes 0.01 mol% to 50 mol% of tetravalent vanadium ions (V 4+ ), and has a thermal expansion coefficient of 65 × 10 −7. It provides a frit composition for sealing an electrical device panel including 60 to 95% by weight of the mother glass and 5 to 40% by weight of filler in the range of / ℃ to 95 x 10 -7 / ℃.
In addition, the present invention, the mother glass further includes P 2 O 5 15 to 35 mol%, ZnO 15 to 25 mol%, Bi 2 O 3 3 to 20 mol%, BaO 1 to 5 mol%, TiO 2 1 to 3 mol%
Provided is a frit composition for sealing an element panel.
In addition, the present invention is a method of adding a vanadium compound of the tetravalent vanadium ions (V 4 + ) containing a) V 4 + ions in the preparation of the frit composition; b) a method of reducing V 5+ ions in V 5+ oxides to V 4+ ions by adding a V 5+ oxide and a reducing agent in preparing the mother glass; c) providing a frit composition for sealing an electrical device panel, wherein the frit composition including the V 5+ oxide is heat-treated under a reducing atmosphere to generate V 5+ ions to V 4+ ions. do.
In addition, the present invention provides a frit composition for sealing an electrical device panel, characterized in that the reducing agent is represented by the formula R'O (the R '= Sn or Cu) and added in a range of 0.1 to 5 mol%.
In addition, the present invention provides an electrical device sealed using the frit composition for sealing the electrical device panel.
When the solar cell panel is sealed using the frit composition for sealing the electric device panel of the present invention, it is effective in preventing moisture or oxygen penetration and has excellent chemical resistance against electrolyte and high absorption rate for electromagnetic waves in the wavelength range of 200 nm to 10,000 nm. Suitable for sealing
1 is a cross-sectional view of a dye-sensitized solar cell device of the electric device according to the present invention
Figure 2 is a conceptual diagram of the manufacturing of the electrical device through the laser sealing method according to the present invention
Figure 3 is a photomicrograph before and after sintering of the first substrate, the second substrate through a laser sealing method according to the present invention
Figure 4 is a graph of the thermal analysis of the paste composition prepared in the embodiment of the present invention
Hereinafter, the present invention will be described in detail with reference to the drawings attached hereto.
In the present specification, terms such as 'laser' or 'laser encapsulation' refer to a light source capable of irradiating electromagnetic waves having a wavelength of 200 to 10,000 nm, such as a laser or an optical lamp, or an encapsulation method using the light source.
1 is a cross-sectional view of a dye-sensitized solar cell device of the electric device according to the present invention. As can be seen in Figure 1, the frit composition for sealing the electrical device panel of the present invention is used as the sealing material of the electrical device panel, and comprises 0.01 mol% to 50 mol% of tetravalent vanadium ions (V 4 + ) And 60 to 95% by weight of the base glass and 5 to 40% by weight of the filler having a coefficient of thermal expansion ranging from 65 × 10 −7 / ° C. to 95 × 10 −7 / ° C.
The mother glass of the frit composition for sealing an electric device of the present invention contains 0.01 mol% to 50 mol% of tetravalent vanadium ions (V 4+ ). Vanadium ions are generally present in the form of V 2 O 5, an oxide of V 5 + which is a pentavalent cation. The V 5 +, which is a pentavalent cation, is in the range of 200 nm to 10,000 nm, which is a light source used for sealing such as a laser or an optical lamp. Absorption rate for the electromagnetic wave having is lower than that of tetravalent vanadium ions (V 4+ ). Therefore, in the present invention, tetravalent vanadium ions in the mother glass may be included in a range of 0.01 mol% to 50 mol% to effectively absorb electromagnetic waves having a wavelength in the range of 200 nm to 10,000 nm. The tetravalent vanadium ions (V 4+ ) are a) a method of adding a vanadium compound including a V 4+ ion in the preparation of the frit composition; b) a method of reducing V 5+ ions in V 5+ oxides to V 4+ ions by adding a V 5+ oxide and a reducing agent in preparing the mother glass; c) A frit composition comprising a V 5+ oxide may be produced by any of the methods of reducing the V 5+ ions to V 4+ ions by heat treatment in a reducing atmosphere.
The tetravalent vanadium ions (V 4+ ) is preferably included in the range of 0.01 mol% to 50 mol% based on the entire mother glass. When the content of tetravalent vanadium ions (V 4+ ) is less than 0.01 mol%, the absorption efficiency of electromagnetic waves is low, so that the effect of addition is insignificant. On the other hand, when the content of the tetravalent vanadium ions (V 4+ ) exceeds 50 mol%, the amount of tetravalent vanadium ions is too high. This is because other characteristics may deteriorate.
In the frit composition for sealing an electrical device panel of the present invention, the mother glass is P 2 O 5 15 to 35 mol%, ZnO 15 to 25 mol%, Bi 2 O 3 3 to 20 mol%, BaO 1 to 5 mol% and TiO 2 1 to 3 mol It may further include%. For the description of the role and the critical significance of the numerical values of the above components, reference may be made to the matters described in the applicant's patent applications 10-2008-0111935 and 10-2009-0110163.
The frit composition for sealing an electrical device panel of the present invention may be expanded in volume while being softened by electromagnetic wave irradiation. In this case, it may be difficult to obtain a sealing material having excellent sealing properties. Therefore, the frit composition for sealing an electrical device of the present invention includes a filler capable of lowering the coefficient of thermal expansion in a range of 5 to 40 wt% based on the total weight of the entire frit composition. Specific examples of the filler include zirconium-tungsten-phosphate fillers, zirconium-phosphate fillers (e.g. zirconium phosphate), zirconium fillers (e.g. zirconia), and eutectic fillers (e.g. Tight), cordierite-based fillers, alumina, silica, zinc silicate, aluminum titanate, and the like, but are not limited thereto. More preferably, for the zirconium-tungsten-phosphate filler, for example, (Zr 2 (WO 4 ) (PO 4 ) 2 ), and cordierite, for example, 5SiO 2 · 3MgO 3Al 2 O It may be 3 but is not limited thereto. The filler that may be included in the composition for forming a sealing material as described above is preferably softened by laser irradiation, and in consideration of this, the average particle diameter of the filler may be 0.1 μm to 30 μm, preferably 0.5 μm to 15 μm. .
The thermal expansion coefficient of the frit composition for sealing an electrical device panel of the present invention is 65 x 10 -7 / ℃ to 95 x 10 -7 / ℃, more preferably 75 x 10 -7 / ℃ to 85 x 10 -7 / ℃ Can be. The thermal expansion coefficient of the above range can be prevented between the substrate mismatch due to the volume change by the electromagnetic wave irradiation when the electrical device panel is sealed.
Meanwhile, the frit composition for sealing an electrical device panel of the present invention may be processed into a paste form by mixing with an organic vehicle to obtain proper printability, viscosity, and flowability. The organic vehicle may be an organic material so that it may decompose upon heat treatment. For example, the vehicle may include a resin and a solvent. The resin may be, for example, one or more resins selected from the group consisting of acrylic resins, methacryl resins, and vinyl resins, but is not limited thereto. The solvent may be one or more selected from the group consisting of terpinol, dihydro trrpinol, butylcarbitolacetatr, and butyl carbitol, but is not limited thereto. .
The content of the vehicle may be selected in consideration of printability, viscosity, flowability, etc. of the frit composition for sealing the electrical device panel, for example, 10 to 60 parts by weight per 100 parts by weight of the frit composition for sealing the electrical device panel Parts, preferably kneaded in a range of 20 parts by weight to 50 parts by weight, to prepare a paste.
The paste is applied to the adhesive side of the electrical device panel and dried. The drying temperature and time are selected to a temperature and a time range in which the solvent of the vehicle in the paste can be decomposed, and it is preferable that the organic matter inside the panel is not decomposed. In consideration of this, the heat treatment temperature and time may be selected in the range of 50 ℃ to 250 ℃, preferably 80 ℃ to 250 ℃ and 5 minutes to 240 minutes, preferably 10 minutes to 120 minutes.
On the other hand, the frit composition for sealing the electrical device panel is sealed after drying the paste using a laser or an optical lamp. Since the laser or the optical lamp is capable of irradiating the electromagnetic wave locally to the sealing material forming region, the organic material element 13 of the electrical device panel 10 may not be substantially deteriorated when the sealing
Hereinafter, the present invention will be described in more detail with reference to examples of the present invention. However, the following examples are only for understanding the present invention, but the scope of the present invention is not limited to the following examples.
Example 1 (preparation of frit composition)
Each glass powder was prepared in the composition shown in Table 1 below. First, batch raw materials were combined to have the composition shown in Table 1 and melted for 10 to 30 minutes at a temperature of 1160 ° C. in air. Next, the molten glass was passed through a roller to form a thin plate, and ball milled to prepare a frit. The flow button was measured on a schedule of 15 minutes at 450 ℃ for 15 minutes at a temperature of 7.7 ℃ per minute, and the spreadability of frit was matched with the substrate glass.
(w / t%)
-
-
7.0
(x10-7 /)
◎: Good overall adhesive strength ○: Good adhesive strength Δ: Poor adhesion
As can be seen in the above embodiment, in the case of the composition 1, the size of the flow button was appropriate, but the adhesive form was not evenly sealed on the entire surface of the substrate. In addition, in the case of composition 2, the adhesive force adhered well over the board | substrate. In the case of composition 3, the size of the flow button was the largest, but the adhesive form was not evenly sealed on the entire surface of the substrate. Composition 4 and 5 had good flow button size and good adhesion. In particular, in the case of composition 5, the adhesion was the best. Therefore, in Example 1, it can be seen that the composition 5 has F / B, Tg, and Ts which are easy for baking at 450 ° C.
Example 2 (Preparation and Sealing of Paste Composition)
An organic vehicle was prepared by mixing 30 parts by weight of butyl carbitol acetate and 70 parts by weight of terpineol, and then mixing 70 parts by weight of the solvent and 30 parts by weight of elbasite, an acrylate polymer, as a binder. A glass encapsulant paste composition was prepared by mixing 25 parts by weight of the organic vehicle and 75 parts by weight of a frit having the composition of Preparation Example. The prepared sealing paste composition was dispensed quantitatively on a general soda lime front substrate by a dispensing method, and dried. The adhesion state of the upper and lower plate glass substrates of the sealing layer was about 20 to 60 μm in a line width of 3 to 6 mm, and the firing characteristics of the paste composition were confirmed using a TG-DTA thermal analyzer. 4 is a thermal analysis result of the paste composition prepared in the above embodiment. As shown in FIG. 4, in the case of a paste prepared by kneading the frit composition for sealing a dye-sensitized solar cell panel of the present invention with an organic vehicle, it can be seen that the binder is completely decomposed at around 250 ° C., which is suitable for low temperature exhaust.
Example 3 (laser sealing)
The frit composition formed in Example 2 was sealed using an laser equipment by adjusting the power and irradiation speed of the laser beam. The power of the laser beam was adjusted to 30 watts and the irradiation speed was 150 mm / sec to complete the dye-sensitized solar cell through laser sealing.
The result of the sealing performed in Example 3 was confirmed by optical microscope and thermal analysis. As can be seen in Figure 3, when dispensing the above-mentioned paste composition was well formed of the line by adjusting the appropriate viscosity, even when sealed by firing using a real laser that is well sealed throughout the whole period I could confirm
One embodiment of the present invention described above should not be construed as limiting the technical spirit of the present invention. The scope of protection of the present invention is limited only by the matters described in the claims, and those skilled in the art will be able to modify the technical idea of the present invention in various forms. Accordingly, such improvements and modifications will fall within the scope of the present invention as long as they are obvious to those skilled in the art.
Claims (5)
The mother glass further comprises 15 to 35 mol% of P 2 O 5, 15 to 25 mol% of ZnO, 3 to 20 mol% of Bi 2 O 3 , 1 to 5 mol% of BaO and 1 to 3 mol% of TiO 2. .
The tetravalent vanadium ions (V 4+ ) are a) a method of adding a vanadium compound including a V 4+ ion in the preparation of the frit composition; b) a method of reducing V 5+ ions in V 5+ oxides to V 4+ ions by adding a V 5+ oxide and a reducing agent in preparing the mother glass; c) A frit composition for sealing an electric device panel, wherein the frit composition including the V 5+ oxide is heat-treated under a reducing atmosphere to reduce V 5+ ions to V 4+ ions.
The reducing agent is represented by the formula R'O (the R '= Sn or Cu) and the frit composition for sealing the electrical device panel, characterized in that added in the range of 0.1 to 5 mol%.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| KR1020120058166A KR20130134564A (en) | 2012-05-31 | 2012-05-31 | Frit composition for sealing electric component panels and electric components sealed with said frit composition |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| KR1020120058166A KR20130134564A (en) | 2012-05-31 | 2012-05-31 | Frit composition for sealing electric component panels and electric components sealed with said frit composition |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR20150136359A (en) * | 2014-05-27 | 2015-12-07 | 공주대학교 산학협력단 | Sealing frit composition for oled display with enhanced adhesion and paste composition containing the same |
| KR20180013516A (en) * | 2016-07-29 | 2018-02-07 | 공주대학교 산학협력단 | Glass materials for large scale dye-sensitized solar cell sealing and pastes comprising the same |
| WO2024063440A1 (en) * | 2022-09-23 | 2024-03-28 | 주식회사 베이스 | Lead-free low-temperature fired glass frit |
-
2012
- 2012-05-31 KR KR1020120058166A patent/KR20130134564A/en not_active Application Discontinuation
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR20150136359A (en) * | 2014-05-27 | 2015-12-07 | 공주대학교 산학협력단 | Sealing frit composition for oled display with enhanced adhesion and paste composition containing the same |
| KR20180013516A (en) * | 2016-07-29 | 2018-02-07 | 공주대학교 산학협력단 | Glass materials for large scale dye-sensitized solar cell sealing and pastes comprising the same |
| WO2024063440A1 (en) * | 2022-09-23 | 2024-03-28 | 주식회사 베이스 | Lead-free low-temperature fired glass frit |
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