TWI388039B - 密封技術及密閉性地密封元件 - Google Patents
密封技術及密閉性地密封元件 Download PDFInfo
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- TWI388039B TWI388039B TW097122801A TW97122801A TWI388039B TW I388039 B TWI388039 B TW I388039B TW 097122801 A TW097122801 A TW 097122801A TW 97122801 A TW97122801 A TW 97122801A TW I388039 B TWI388039 B TW I388039B
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- 238000000034 method Methods 0.000 title claims description 52
- 238000007789 sealing Methods 0.000 title claims description 50
- 239000000463 material Substances 0.000 claims description 97
- 239000003566 sealing material Substances 0.000 claims description 45
- 239000000758 substrate Substances 0.000 claims description 32
- 238000000151 deposition Methods 0.000 claims description 29
- 229910052809 inorganic oxide Inorganic materials 0.000 claims description 27
- GCFDVEHYSAUQGL-UHFFFAOYSA-J fluoro-dioxido-oxo-$l^{5}-phosphane;tin(4+) Chemical compound [Sn+4].[O-]P([O-])(F)=O.[O-]P([O-])(F)=O GCFDVEHYSAUQGL-UHFFFAOYSA-J 0.000 claims description 26
- 238000001816 cooling Methods 0.000 claims description 20
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 14
- 238000010438 heat treatment Methods 0.000 claims description 14
- 239000011147 inorganic material Substances 0.000 claims description 14
- 239000001301 oxygen Substances 0.000 claims description 14
- 229910052760 oxygen Inorganic materials 0.000 claims description 14
- 229910010272 inorganic material Inorganic materials 0.000 claims description 13
- 239000002019 doping agent Substances 0.000 claims description 8
- 239000010409 thin film Substances 0.000 claims description 7
- 229910019142 PO4 Inorganic materials 0.000 claims description 6
- 239000010452 phosphate Substances 0.000 claims description 6
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 claims description 6
- BTBUEUYNUDRHOZ-UHFFFAOYSA-N Borate Chemical compound [O-]B([O-])[O-] BTBUEUYNUDRHOZ-UHFFFAOYSA-N 0.000 claims description 5
- 239000000203 mixture Substances 0.000 claims description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 4
- 238000004519 manufacturing process Methods 0.000 claims description 3
- 230000035699 permeability Effects 0.000 claims description 3
- 239000000126 substance Substances 0.000 claims description 3
- GRXSUGFAJHRXIP-UHFFFAOYSA-F P(=O)([O-])([O-])F.[W+4].[Sn+4].P(=O)([O-])([O-])F.P(=O)([O-])([O-])F.P(=O)([O-])([O-])F Chemical compound P(=O)([O-])([O-])F.[W+4].[Sn+4].P(=O)([O-])([O-])F.P(=O)([O-])([O-])F.P(=O)([O-])([O-])F GRXSUGFAJHRXIP-UHFFFAOYSA-F 0.000 claims description 2
- 239000013078 crystal Substances 0.000 claims description 2
- 239000003814 drug Substances 0.000 claims description 2
- 229940079593 drug Drugs 0.000 claims description 2
- 239000011261 inert gas Substances 0.000 claims description 2
- 230000003287 optical effect Effects 0.000 claims description 2
- 229920000642 polymer Polymers 0.000 claims description 2
- 230000035945 sensitivity Effects 0.000 claims description 2
- YZYDPPZYDIRSJT-UHFFFAOYSA-K boron phosphate Chemical compound [B+3].[O-]P([O-])([O-])=O YZYDPPZYDIRSJT-UHFFFAOYSA-K 0.000 claims 2
- 229910000149 boron phosphate Inorganic materials 0.000 claims 2
- 150000004770 chalcogenides Chemical class 0.000 claims 2
- XNGIFLGASWRNHJ-UHFFFAOYSA-L phthalate(2-) Chemical compound [O-]C(=O)C1=CC=CC=C1C([O-])=O XNGIFLGASWRNHJ-UHFFFAOYSA-L 0.000 claims 2
- QHGNHLZPVBIIPX-UHFFFAOYSA-N tin(II) oxide Inorganic materials [Sn]=O QHGNHLZPVBIIPX-UHFFFAOYSA-N 0.000 description 24
- 230000008021 deposition Effects 0.000 description 18
- 239000010408 film Substances 0.000 description 13
- 238000012360 testing method Methods 0.000 description 12
- 239000011575 calcium Substances 0.000 description 11
- 238000004544 sputter deposition Methods 0.000 description 10
- 229910052791 calcium Inorganic materials 0.000 description 9
- 230000004888 barrier function Effects 0.000 description 8
- 230000008569 process Effects 0.000 description 8
- 239000000843 powder Substances 0.000 description 7
- 239000005303 fluorophosphate glass Substances 0.000 description 6
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 5
- 229910052782 aluminium Inorganic materials 0.000 description 5
- 230000008859 change Effects 0.000 description 5
- 239000011521 glass Substances 0.000 description 5
- 229910008449 SnF 2 Inorganic materials 0.000 description 4
- 239000011248 coating agent Substances 0.000 description 4
- 238000000576 coating method Methods 0.000 description 4
- 230000007547 defect Effects 0.000 description 4
- 230000008901 benefit Effects 0.000 description 3
- 238000006731 degradation reaction Methods 0.000 description 3
- 238000005538 encapsulation Methods 0.000 description 3
- 239000011368 organic material Substances 0.000 description 3
- 239000005365 phosphate glass Substances 0.000 description 3
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 2
- 230000032683 aging Effects 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 239000005385 borate glass Substances 0.000 description 2
- 230000015556 catabolic process Effects 0.000 description 2
- 239000003054 catalyst Substances 0.000 description 2
- 239000005387 chalcogenide glass Substances 0.000 description 2
- 239000000975 dye Substances 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000001704 evaporation Methods 0.000 description 2
- 230000008020 evaporation Effects 0.000 description 2
- 230000007246 mechanism Effects 0.000 description 2
- 230000008018 melting Effects 0.000 description 2
- 238000002844 melting Methods 0.000 description 2
- 238000000059 patterning Methods 0.000 description 2
- 230000002829 reductive effect Effects 0.000 description 2
- 239000005361 soda-lime glass Substances 0.000 description 2
- 238000007736 thin film deposition technique Methods 0.000 description 2
- 230000008016 vaporization Effects 0.000 description 2
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 description 1
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 1
- 229910005728 SnZn Inorganic materials 0.000 description 1
- 241000532412 Vitex Species 0.000 description 1
- 229910052783 alkali metal Inorganic materials 0.000 description 1
- 150000001340 alkali metals Chemical class 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 238000000137 annealing Methods 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 239000006229 carbon black Substances 0.000 description 1
- 238000005266 casting Methods 0.000 description 1
- 239000010406 cathode material Substances 0.000 description 1
- 235000009347 chasteberry Nutrition 0.000 description 1
- 238000010549 co-Evaporation Methods 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 238000007596 consolidation process Methods 0.000 description 1
- 230000000593 degrading effect Effects 0.000 description 1
- 230000032798 delamination Effects 0.000 description 1
- 230000006866 deterioration Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000003618 dip coating Methods 0.000 description 1
- XPPKVPWEQAFLFU-UHFFFAOYSA-J diphosphate(4-) Chemical compound [O-]P([O-])(=O)OP([O-])([O-])=O XPPKVPWEQAFLFU-UHFFFAOYSA-J 0.000 description 1
- 235000011180 diphosphates Nutrition 0.000 description 1
- 239000000428 dust Substances 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 239000003822 epoxy resin Substances 0.000 description 1
- 230000003628 erosive effect Effects 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 239000007888 film coating Substances 0.000 description 1
- 238000009501 film coating Methods 0.000 description 1
- 229910052731 fluorine Inorganic materials 0.000 description 1
- 239000011737 fluorine Substances 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 229910001385 heavy metal Inorganic materials 0.000 description 1
- 230000003301 hydrolyzing effect Effects 0.000 description 1
- AMGQUBHHOARCQH-UHFFFAOYSA-N indium;oxotin Chemical compound [In].[Sn]=O AMGQUBHHOARCQH-UHFFFAOYSA-N 0.000 description 1
- 239000012212 insulator Substances 0.000 description 1
- 238000000608 laser ablation Methods 0.000 description 1
- 230000000670 limiting effect Effects 0.000 description 1
- 230000005923 long-lasting effect Effects 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 230000000873 masking effect Effects 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 238000005457 optimization Methods 0.000 description 1
- 238000013086 organic photovoltaic Methods 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 238000004806 packaging method and process Methods 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 230000035515 penetration Effects 0.000 description 1
- 239000012466 permeate Substances 0.000 description 1
- 238000009512 pharmaceutical packaging Methods 0.000 description 1
- 229910052698 phosphorus Inorganic materials 0.000 description 1
- 239000011574 phosphorus Substances 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 229920000647 polyepoxide Polymers 0.000 description 1
- 239000002861 polymer material Substances 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 239000002096 quantum dot Substances 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 238000005546 reactive sputtering Methods 0.000 description 1
- 238000005096 rolling process Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 239000005368 silicate glass Substances 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 150000003384 small molecules Chemical class 0.000 description 1
- 238000004528 spin coating Methods 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- 230000001629 suppression Effects 0.000 description 1
- SITVSCPRJNYAGV-UHFFFAOYSA-L tellurite Chemical compound [O-][Te]([O-])=O SITVSCPRJNYAGV-UHFFFAOYSA-L 0.000 description 1
- 238000000427 thin-film deposition Methods 0.000 description 1
- 238000007740 vapor deposition Methods 0.000 description 1
- 238000009834 vaporization Methods 0.000 description 1
- 239000006200 vaporizer Substances 0.000 description 1
- 239000010455 vermiculite Substances 0.000 description 1
- 229910052902 vermiculite Inorganic materials 0.000 description 1
- 235000019354 vermiculite Nutrition 0.000 description 1
- 238000009736 wetting Methods 0.000 description 1
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- H—ELECTRICITY
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- H10K71/10—Deposition of organic active material
- H10K71/16—Deposition of organic active material using physical vapour deposition [PVD], e.g. vacuum deposition or sputtering
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
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- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
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- C03—GLASS; MINERAL OR SLAG WOOL
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- C03C17/00—Surface treatment of glass, not in the form of fibres or filaments, by coating
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- C03C17/3602—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions at least one coating being a metal the metal being present as a layer
- C03C17/3615—Coatings of the type glass/metal/other inorganic layers, at least one layer being non-metallic
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- 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
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- C03C17/00—Surface treatment of glass, not in the form of fibres or filaments, by coating
- C03C17/34—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions
- C03C17/36—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions at least one coating being a metal
- C03C17/3602—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions at least one coating being a metal the metal being present as a layer
- C03C17/3668—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions at least one coating being a metal the metal being present as a layer the multilayer coating having electrical properties
- C03C17/3671—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions at least one coating being a metal the metal being present as a layer the multilayer coating having electrical properties specially adapted for use as electrodes
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- C—CHEMISTRY; METALLURGY
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- 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
- C03C17/00—Surface treatment of glass, not in the form of fibres or filaments, by coating
- C03C17/34—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions
- C03C17/36—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions at least one coating being a metal
- C03C17/3602—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions at least one coating being a metal the metal being present as a layer
- C03C17/3668—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions at least one coating being a metal the metal being present as a layer the multilayer coating having electrical properties
- C03C17/3678—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions at least one coating being a metal the metal being present as a layer the multilayer coating having electrical properties specially adapted for use in solar cells
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- C—CHEMISTRY; METALLURGY
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- C03C3/00—Glass compositions
- C03C3/12—Silica-free oxide glass compositions
- C03C3/23—Silica-free oxide glass compositions containing halogen and at least one oxide, e.g. oxide of boron
- C03C3/247—Silica-free oxide glass compositions containing halogen and at least one oxide, e.g. oxide of boron containing fluorine and phosphorus
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- 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
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- H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
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- H10K50/80—Constructional details
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- Structures Or Materials For Encapsulating Or Coating Semiconductor Devices Or Solid State Devices (AREA)
Description
本發明係關於密封方法以減小密閉性密封元件所需要時間以及產生密閉性密封元件。密閉性密封元件之範例包含發光元件(例如有機發光二極體(OLED)元件),光伏打元件,薄膜感測器,瞬逝波導感測器,食物容器及藥品容器。
氧氣或水份傳移通過疊層或包封材料及後續侵蝕元件內部材料代表許多元件兩種較普遍相關之衰變機制,該元件例如為發光元件(OLED元件),薄膜感測器,及瞬逝波導感測器,食物容器及藥品容器。為了詳細說明關於氧氣及水份滲透至OLED及其他元件之內層(陰極及電-發冷光材料)問題,可參考下列文獻:
Aziz,H.,Popovic,Z.D.,Hu,N.X.,Hor,A.H.,and Xu,G."Degradation Mechanism of Small Molecule - Based Organic Light - Emitting Devices",Science,283,pp.1900 - 1902,(1999)。
Burrows,P.E.,Bulovic.,V.,Forrest,S.R.,Sapochak,L.S., McCarty,D.M.,Thompson,M.E."Reliability and Degradation of Organic Light Emitting Devices",Applied Physics Letters,65(23),pp.2922 - 2924。
Kolosov,D.,et al.,Direct observation of structural changes in organic light emitting devices during degrada - tion.Journal of Applied Physics,1001.90(7)。
Liew,F.Y.,et al.,Investigation of the sites of dark spots in organic light - emitting devices.Applied Physics Letters,1000.77(17)。
Chatham,H.,"Review:Oxygen Diffusion Barrier Properties of Transparent Oxide Coatings on Polymeric Substrates",78,pp.1 - 9,(1996)。
人們了解除非完成一些處置使氧氣及水份滲透至OLED元件減為最低程度,該元件操作壽命將受到嚴重限制。已作許多嘗試使氧氣以及水份滲透至OLED元件以及有助於促使OLED操作壽命朝向4萬小時,其通常視為必要的,使OLED元件能夠超過舊的例如LCD顯示器技術,其在下面文獻中已作說明:Forsythe,Eric,W.之"Operation of Organic - Based Light - Emitting Devices",in Society for Information Display(SID)40th
anniversary Seminar Lecture Notes,Vol.1,Seminar M5,Hynes Convention Center,Boston,MA,May 20 and 24,(2002)。
至目前進行更積極的嘗試以有助於延長OLED元件之使用壽命包含使用吸氣劑,包封及廣泛元件之密封技術。實際上,目前一項常用密封OLED元件之方法為塗覆以及熱處理(或紫外線)不同形式之環氧樹脂,無機材
料及/或有機材料以形成密封於OLED元件上。例如,Vitex系統製造及銷售商標名稱為Barix之複合物形式塗膜,其中無機材料及有機材料交替層使用來密封OLED元件。雖然這些形式密封提供某種程度密閉特性,其為昂貴的以及存在許多情況無法在長期操作情況下防止氧氣及水份擴散進入OLED元件。
為了解決該密封問題,本公司已發展數種不同的密封技術,其中密封材料(例如低液相線溫度無機材料,含Sn2+
無機氧化物材料)使用來密閉性密封OLED元件(或其他型式元件)(參閱先前所提及美國第11/207691及11/803512號專利申請案)。雖然這些密封技術以及密封材料運作良好以密閉性密封OLED元件(或其他形式之元件),仍然需要對這些密封技術作改善,使得人們能夠減少密閉性密封OLED元件(或其他形式元件)所需要時間。該特別需求以及其他需求可藉由本發明得到令人滿意結果。
本發明說明一種減少密閉性密封元件(例如OLED元件)所需要時間之方法。密封方法包含下列步驟:(1)冷卻未經包封元件;(2)沉積密封材料於經冷卻元件的至少部份以形成經包封元件;以及(3)熱處理經包封元件以形成密閉性密封元件。在一項實施例中,密封材料為低
液相線溫度無機(LLT)材料,例如錫-氟磷酸鹽玻璃,摻雜鎢之錫-氟磷酸鹽玻璃,硫屬化物玻璃,碲酸鹽玻璃,硼酸鹽玻璃及磷酸鹽玻璃。在另一項實施例中,密封材料為含Sn2+
無機氧化物材料例如為SnO,SnO+P2
O5
以及SnO+BPO4
。使用該密封方法之優點在於藉由冷卻未經經包封元件,因而能夠增加沉積速率,密封材料(例如LLT材料含Sn2+
無機氧化物材料)沉積於未經包封元件上,其將減少密閉性密封元件(例如OLED元件)所需要時間。
參考圖1-2,其分別地顯示出密閉性密封元件100之斷面側視圖以及密封方法200之流程圖,其使用來製造依據本發明之密閉性密封元件100。如圖1所示,密閉性密封元件100包含熱處理材料102(例如熱處理低液相線溫度無機材料102或熱處理含Sn2+
無機氧化物材料102),其包封以及密閉性密封一個或多個位於支撐/基板106上內層/組件104。
圖2示意性地顯示出具有步驟202,204及206之密封方法200。密封方法200具有冷卻步驟202,其中基板106以及未經包封元件100之內層/組件104冷卻至溫度為:較佳為<15℃,更佳為<10℃以及最佳為<1℃。除此,密封方法200具有沉積步驟204,其中密封材料102(例
如LLT材料102或含Sn2+
無機氧化物材料102)沉積於位於冷卻支撐/基板106頂部上內層/組件104上方。在一項實施例中,密封材料102能夠沉積於冷卻內層/組件104以及冷卻支撐/基板106上,沉積速率例如為:較佳地約為5埃/秒,更佳地約為25埃/秒,以及最佳地約為75埃/秒。加上,密封材料102能夠使用任何不同的處理過程加以沉積,包含:例如濺鍍,快速蒸鍍,噴鍍,澆注,玻璃料沉積,汽相沉積,浸漬塗覆,刷塗,滾塗(例如使用密封材料102薄膜),旋轉塗覆,共同蒸鍍處理過程,粉塵槍噴鍍處理過程,反應濺鍍處理過程,雷射剝蝕處理過程,或其組合。
除此,密封方法200具有熱處理步驟206,其中經包封元件100加以退火,固結或熱處理(例如在小於100℃小於3小時)以形成密閉性密封元件100。進行熱處理步驟206在沉積密封材料102內去除缺陷(例如孔隙)/使缺陷減為最低,該缺陷在沉積步驟204過程中形成(注意:假如使用含Sn2+
無機氧化物材料102,且特別是SnO,則以再濺鍍沉積步驟204本身提供燒結沉積材料102所有熱量)。在一項實施例中,經包封元件100能夠在下列溫度下進行熱處理(例如):較佳為<400℃,更佳為<200℃,更佳為<100℃,以及最佳為<40℃。假如需要情況下,冷卻步驟202,沉積步驟204以及熱處理步驟206全部能夠在惰性氣體或真空中進行以有助於確保在整個密封處理過程中保持無水份及氧情況。該形式處理環境有助
於確保位於密閉性密封元件100內之有機電子產物104強固,長使用壽命操作。
密封方法200主要優點在於藉由冷卻未經包封元件100能夠增加密封材料102沉積於未經包封元件100之沉積速率,其減少密閉性密封元件100所需要時間。當人們想要大量操作以及製造大量密閉性密封元件100時,該沉積速率為重要的。密閉性密封元件100之範例包含發光元件(例如為OLED元件),光伏打元件,薄膜感測器,瞬逝波導感測器,食物容器及藥品容器。
假如人們製造OLED元件100,則內層104包含陰極以及電發光材料,其兩者位於基板106上。這些陰極以及電發光材料104假如加熱高於例如100-125℃將會受到損壞。因而,假如傳統材料(例如為蘇打-石灰玻璃)沉積於OLED元件100上熱處理步驟206在該特別應用中將為不可能的。由於,在傳統材料中(例如蘇打-石灰玻璃)中去除缺陷所需要之溫度(例如600℃)將太高以及因而嚴重地損壞OLED元件之內層104。不過,在本發明中,在該特別應用中熱處理步驟206能夠實施於該特別應用中,因為去除/減少存在於沉積密封材料102中缺陷所需要溫度(例如為100℃或更低)為相當低而不會損及OLED元件之內層104。為了達成該情況,使用來包封經冷卻元件100之密封材料102優先地為低液相線溫度(LLT)無機材料102或含Sn2+
無機氧化物材料102。這些密封材料簡單地說明於底下,但是更詳細地說明於美
國第11/207691及11/803512號專利中。
LLT材料102能夠達成該情況,因為該形式材料具有相對低的液相線溫度≦1000℃。低液相線溫度係指LLT 102能夠在相當低溫度下熱處理,其並不會以熱力損及OLED內層104,仍然導致無孔隙薄膜形成於OLED元件100上。再次地,人們了解熱處理LLT材料102能夠使用作為障壁層,其在廣泛種類元件100以及OLED元件100例如為薄膜感測器,光伏打元件,瞬逝波導感測器,食物容器,藥品容器或任何形式之電子元件上,其對水氣,氧氣或其他氣體為靈敏的(注意:在此亦能夠使用另一LLT材料102即摻雜鎢錫氟磷酸鹽玻璃以及該材料揭示於相關美國第11/544262號專利申請案中,該專利之說明在此加入作為參考)。
在一項實施例中,LLT材料102為低液相線溫度≦1000℃(以及更佳為≦600℃以及最佳為≦400℃)。LLT材料102包含例如玻璃例如為錫氟磷酸鹽玻璃,摻雜鎢之錫-氟磷酸鹽玻璃,硫屬化物玻璃,碲酸鹽玻璃,硼酸鹽玻璃以及磷酸鹽玻璃(例如為鹼金屬Zn或SnZn焦磷酸鹽)。例如,優先地錫氟磷酸鹽玻璃具有下列組成份:Sn(20-85重量百分比),P(2-20重量百分比),O(10-36重量百分比),F(10-36重量百分比),Nb(0-5重量百分比)以及Sn+P+O+F至少為75%(其能夠熔融粉末標的物或濺鍍緊壓粉末標的)。這些LLT材料102基於數種不同理由為需要的,其包含(例如):
LLT材料102能夠不含重金屬以及其他環境上不想要之材料。
LLT材料102為耐久性的以及當浸漬於85℃水中呈現出低溶解的。
LLT材料102能夠含有染料分子以及能夠摻雜高達8mM(4.8x1018
/cm3
)數量。
LLT磷酸鹽玻璃氦滲透係數小於熔融矽石情況4至5數量等級。
除此,含Sn2+
無機氧化物材料102能夠使上述情況為可能的,因為該形式材料在相當低溫度下具有形成保護元件100包封塗膜之能力。含Sn2+
無機氧化物材料102在數項目與錫氟磷酸鹽材料不相同,該材料為一項先前所提及LLT材料。首先,含Sn2+
無機氧化物材料102能夠在相當低溫度下進行熱處理而低於錫氟磷酸鹽材料(注意:底下對圖3-4所說明特定錫氟磷酸鹽材料能夠在約120℃下進行熱處理)。其次,含Sn2+
無機氧化物材料102並不含氟。第三,一些含Sn2+
無機氧化物材料102例如為SnO之熔融溫度超過1000℃,其大於錫氟磷酸鹽材料相關最高熔融溫度1000℃。第四,當與錫氟磷酸鹽材料作比較時,含Sn2+
無機氧化物材料102具有不同的組成份。
含Sn2+
無機氧化物材料102包含組成份例如SnO粉末,混合SnO/含P2
O5
粉末(例如為80% SnO+20% P2
O5
),以及混合SnO/含P2
O5
粉末(例如為90% SnO+10%
P2
O5
)。不過,含Sn2+
無機氧化物材料102亦能夠包含混合組成份,其被熔融形成適當的濺鍍標的(例如80% SnO+20% P2
O5
)。在一項實施例中,含Sn2+
無機氧化物材料102包含:(1)SnO;(2)SnO及硼酸鹽材料;(3)SnO及磷酸鹽材料;以及(4)SnO及硼磷酸鹽材料。一般,含Sn2+
無機氧化物材料102能夠含有>50%氧化亞錫(以及優先地>70%氧化亞錫以及更優先地>80%氧化亞錫)。除此,含Sn2+
無機氧化物材料102能夠在<400℃下作熱處理(以及優先地在<200℃下作熱處理以及更優先地在<100℃下作熱處理)。
參考圖3,其為85℃/85%相對濕度加速時效槽/烘箱300圖式,其使用來測試三個元件100(鈣薄片)密閉性,該元件使用相同的錫氟磷酸鹽材料102在相同的沉積條件下製造出,除了元件基板106冷卻至不同的溫度。如圖所示,每一測試元件100具有沉積錫氟磷酸鹽材料102,兩內層104(Al及Ca)以及基板106(玻璃基板106)。特別地,每一測試元件100藉由蒸鍍100nm鈣薄膜104於玻璃基板106(本公司編號1737)頂部上製造出。因而,150nm鋁層104被汽化於鈣薄膜104上。使用Al層104,因為其模擬陰極通常使用於製造聚合物發光二極體(PLED)。使用一般"雙床"Cressington汽化器308R(Ted Pelle,CA),以及在Ca及Al汽化過程中玻璃基板106保持於130℃以及10-6
托下。在冷卻至室溫後,解除真空以及取出鈣薄片以及置於於真空乾燥器中運送至
RF濺鍍真空系統,以及加以泵運至第二天以達到10-6
托真空度。
RF濺鍍真空系統具有溫度控制固定器,其使用來冷卻Ca及Al層104以及基板106之溫度(注意:三個測試元件100分別地保持在150℃,44℃及14℃)。錫氟磷酸鹽材料102(在該情況具有組成份為39.6 SnF2
,38.7 SnO,19.9 P2
O5
,1.8 Nb2
O5
百分莫耳比)在相當快速RF粉末沉積條件(約為70W向前/1W反射RF功率)以及高氬壓力下(約為20 sccm)(參閱圖2中步驟204)藉由ONYX-3濺鍍槍(Angstrom Sciences,PA)再濺鍍於Al及Ca層104上。其次,解除真空以及熱處理元件100全部放置於烘箱300中以及保持為85℃以及85%相對濕度。在每一測試元件100中,Ca層104初始地為高度反射之金屬鏡子。假如水份及氧氣滲透過錫氟磷酸鹽材料102,則金屬性Ca 104產生反應以及轉變為不透明白色薄層,其能夠利用光學量測加以數量化以及因而能夠估計經包封元件100能夠在正常大氣條件下理論上操作之時間(注意:關於標準化鈣薄片測試更詳細說明可參閱美國第11/207691號專利申請案)。該特定試驗結果將對圖4所顯示曲線詳細加以說明於底下。
參閱圖4,其為曲線圖,其顯示出三個測試元件100性能,該元件使用相同的錫氟磷酸鹽材料102在相同的沉積條件下製造出,除了每一元件基板106冷卻至不同的溫度。特別地,第一元件100a在基板溫度為150℃下
利用錫氟磷酸鹽材料102進行包封。第二元件100b在基板溫度為44℃下利用錫氟磷酸鹽材料102進行包封。以及,第三元件100c在基板溫度為14℃下利用錫氟磷酸鹽材料102進行包封。試驗結果清楚地顯示出當基板106在高速率沉積步驟204過程中冷卻時濺鍍沉積錫氟磷酸鹽材料102具有極良好的密閉性阻絕特性(第三元件100c可接受特性與第一及第二元件100a及100b無法接受特性比較)。雖然並不預期受限於理論,我們相信基板106冷卻促使濺鍍沉積錫氟磷酸鹽材料102產生較小顆粒尺寸,其因而促使濺鍍沉積錫氟磷酸鹽材料102更快速地燒結以及形成所需要密閉性薄膜於第三元件100c上。加以對比,以85/85測試結果為基準第一及第二元件100a及100b視為未能令人滿意的,因為當錫氟磷酸鹽材料102以較為緩慢速率沉積時在85/85環境中將法維持1000小時,其已說明於美國第11/207691號專利中。
由於先前說明,業界熟知此技術者能夠立即地了解本發明係關於減少密閉性密封元件100(例如為OLED元件100)所需要時間之密封方法200。密封方法200包含下列步驟:(1)冷卻未經包封元件100;(2)沉積密封材料102於經冷卻元件100的至少部份上以形成經包封元件100;以及熱處理經包封元件100以形成密閉性密封元件100。密封材料102為LLT材料或含Sn2+
無機氧化物材料102。假如所需要多層相同的或不同形式之密封材料102能夠沉積於元件100之頂部。如上述所說明,密封
材料102特別地適合作為抑制氧及/或水氣之劣化,為一般廣泛種類元件100包含電子元件,食物容器以及藥品容器之共同問題。除此,密封材料102可使用來減小由於化學活性滲透劑所導致對元件100例如為光化學,水解聚合,以及氧化之損壞。使用密封材料102一些額外的優點以及特性說明如下:
A.密封材料102可使用來配製密閉性薄膜(約為2微米)障壁層,其達成OLED長壽命之操作(<10-6
水份公克/平方米/日),以及可在元件(或基板材料)上以及在一些極低溫度(<40℃)情況下快速地濺鍍沉積以及退火。元件100包含下列非限制性之:
a.有機電子元件
有機發光二極體(OLED);有機光伏打元件(OPV);有機感測器,具有或不具有觸媒;可撓曲平板元件之可撓曲基板;無線射頻識別標籤(RFID);
b.半導體電子元件
發光二極體(LED);光伏打元件(PV);感測器,具有或不具有觸媒;可撓曲平板元件之可撓曲基板;無線射頻識別標籤(RFID);基板材料包含下列非限制性之:
a.聚合物材料
可撓曲平板元件之可撓曲基板;食物包裝;藥品包裝
B.具有這些特殊密封材料102之有機電子元件的密封在固結/熱處理過程中並不需要氧氣或空氣加入至槽內。特別是在低溫(約為40℃)下並不需要氧化來源以達成密封情況促使該密封技術為製造有機電子元件具有吸引力之結果。上述情況特別真實,因為人們熟知氧氣及水氣為氧化還原以及光致退色劣化反應相關之主要劣化反應劑,其負面地影響位於有機電子元件例如OLED內之有機層及/或陰極材料。
C.濺鍍沉積,蒸鍍,以及其他薄膜沉積處理過程可使用來沉積密封材料102。例如,高速率沉積含Sn2+
無機氧化物薄膜102可藉由在含氧環境中汽化金屬錫於例如為塑膠之高速滾動基板上。可加以變化,在氧環境中無功直流濺鍍金屬錫可使用來產生所需要高速率沉積含Sn2+
無機氧化物薄膜於元件100上。實際上,可使用許多不同的薄膜沉積技術以沉積含Sn2+
無機氧化物薄膜102(以及LLT薄膜102)於元件100上。
D.密封材料102能夠與不同的粉末/摻雜劑配料以產生組成份,其設計來在沉積障壁層中達成特定物理-化學特性。
下列為範例性不同摻雜劑,其能夠與密封材料102
混合在沉積障壁層內達成所需要物理-化學特性:
a.不透明-透明性:例如SnO在可見光波長下為不透明,但是可摻雜例如磷酸鹽以產生透明薄膜。
b.折射率:能夠使用摻雜劑例如P2
O5
,BPO4
以及PbF2
以改變密封材料102之折射率以有助於使元件100之光線透射及/或光線引出最佳化。例如,當空氣間隙以折射率相匹配氧化物材料替換時頂部發射之OLED元件100能夠最佳化。
c.熱膨脹係數(CTE):能夠使用摻雜劑例如SnF2
,P2
O5
及PbF2
以改變密封材料102之熱膨脹係數,其能夠有助於使不同形式之脫層最小化,其通常與熱膨脹係數不相匹配問題相關。
d.靈敏性:能夠加入磷,量子點,無機/有機染料以及分子以產生所需要電-光特性,其對元件最佳化為有用的。例如,摻雜劑例如為能夠使用碳黑以改變密封材料102之電-光特性(Fermi值/電阻)以改善密閉性密封元件100之效率(注意:假如Fermi值實質上偏移則此會促使改變障壁層之導電性,其方式類似於已知之銦-錫-氧化物(ITO)系統)。
e.改變溶解性以及界面潤溼性以較佳址黏附:密封材料102摻雜摻雜劑例如SnF2
,能夠改變沉積障壁薄膜之混和性。在需要情況下,該觀念可藉由改變密封材料102表面潤溼能力而更進一步利用作為黏接目的。
f.刮損抵抗性:可使用摻雜劑例如SnO,SnF2
及
PbF2
以在密封材料中產生硬度。
E.圖案化能力:濺鍍沉積,或其他薄膜沉積法能夠使用不同的形成圖案技術例如遮蔽遮罩等以產生具有特定特性之微結構以有助於元件100操作最佳化(例如有機薄膜電晶體(TFT)元件100能夠具有絕緣體閘形成於其上面以有助於達成良好的電壓低限值)。
雖然本發明數個實施例已顯示於附圖及先前之詳細說明中,人們了解本發明並不受限於所揭示實施例,然而能夠作許多再排列,改變以及替代而並不會脫離下列申請專利範圍所界定以及揭示本發明之精神。
100‧‧‧密閉性密封元件
102‧‧‧熱處理材料
104‧‧‧內層/組件
106‧‧‧支撐/基板
200‧‧‧密封方法
202‧‧‧冷卻步驟
204‧‧‧沉積步驟
206‧‧‧熱處理步驟
300‧‧‧烘箱
100a‧‧‧第一元件
100b‧‧‧第二元件
100c‧‧‧第三元件
同時參考下列附圖閱讀本發明說明書將更完全地了解本發明:圖1為依據本發明密閉性密封元件之斷面側視圖;圖2為流程圖,其顯示出依據本發明減少密閉性密封元件所需要時間之密封方法的步驟;圖3為85℃/85%加速時效槽/烘箱之方塊圖,其使用來測試以類似方法配製出三個元件之密閉性,除了其在密封材料沉積過程中具有不同的基板溫度;以及圖4為曲線圖,其顯示出三種以類似方式配製出之測試元件,除了在密封材料沉積過程中三個元件具有不同的基板溫度。
100‧‧‧密閉性密封元件
102‧‧‧熱處理材料
104‧‧‧內層/組件
106‧‧‧支撐/基板
Claims (25)
- 一種減少密閉性密封一元件所需要時間之方法,該方法包含步驟:冷卻一未經包封元件;沉積一密封材料於該經冷卻元件的至少一部份以形成一經包封元件;以及熱處理該經包封元件以形成一密閉性密封元件,其中該密封材料為一低液相線溫度無機材料或一含有Sn2+ 無機氧化物材料。
- 如申請專利範圍第1項之方法,其中該低液相線溫度無機材料為下列其中一項或其任何組合:錫-氟磷酸鹽材料;摻雜鎢錫-氟磷酸鹽材料;硫屬化物材料;碲酸鹽材料;硼酸鹽材料;以及磷酸鹽材料。
- 如申請專利範圍第1項之方法,其中該低液相線溫度無機材料為一錫-氟磷酸鹽材料,其具有下列組成份:Sn(20-85重量百分比)P(2-20重量百分比) O(10-36重量百分比)F(10-36重量百分比)Nb(0-5重量百分比);以及Sn+P+O+F佔總量至少75%。
- 如申請專利範圍第1項之方法,其中該低液相線溫度無機材料具有≦1000℃之液相線溫度。
- 如申請專利範圍第1項之方法,其中該低液相線溫度無機材料具有≦600℃之液相線溫度。
- 如申請專利範圍第1項之方法,其中該低液相線溫度無機材料具有≦400℃之液相線溫度。
- 如申請專利範圍第1項之方法,其中該含Sn2+ 無機氧化物材料為下列其中一項或其任何組合:SnO;SnO以及一硼酸鹽材料;SnO以及一磷酸鹽材料;以及SnO以及一硼磷酸鹽材料。
- 如申請專利範圍第1項之方法,其中該冷卻步驟更進一步包含以下步驟:冷卻該未經包封元件至溫度<15℃。
- 如申請專利範圍第1項之方法,其中該冷卻步驟更進一步包含以下步驟:冷卻該未經包封元件至溫度<10℃。
- 如申請專利範圍第1項之方法,其中該冷卻步驟更進一步包含以下步驟:冷卻該未經包封元件至溫度<1℃。
- 如申請專利範圍第1項之方法,其中該沉積步驟更進一步包含以下步驟:以約5埃/秒的速率沉積該密封材料於該經冷卻元件的至少一部份上。
- 如申請專利範圍第1項之方法,其中該沉積步驟更進一步包含以下步驟:以約25埃/秒的速率沉積該密封材料於該經冷卻元件的至少一部份上。
- 如申請專利範圍第1項之方法,其中該沉積步驟更進一步包含以下步驟:以約75埃/秒的速率沉積該密封材料於該經冷卻元件的至少一部份上。
- 如申請專利範圍第1項之方法,其中該熱處理步驟在一真空中或在一惰性氣體環境中,以及並不會損及在該元件中組件之溫度下進行沉積。
- 如申請專利範圍第1項之方法,其中該熱處理步驟在<400℃之溫度下進行。
- 如申請專利範圍第1項之方法,其中該熱處理步驟在<200℃之溫度下進行。
- 如申請專利範圍第1項之方法,其中該熱處理步驟在<100℃之溫度下進行。
- 如申請專利範圍第1項之方法,其中該熱處理步驟在<40℃之溫度下進行。
- 如申請專利範圍第1項之方法,其中該密閉性密封元件具有小於0.01cc/m2 /大氣/日之氧滲透率以及小於0.01g/m2 /日之水氣滲透率。
- 如申請專利範圍第1項之方法,其中該密封材料係以一摻雜摻雜劑以達成所需要特定物理-化學特性,該特性為下列其中一項或其任何組合:不透明-透明性;折射率;熱膨脹係數(CTE);靈敏性;Fermi值/電阻;溶解性/界面潤溼性;以及硬度。
- 如申請專利範圍第1項之方法,其中該元件係選自於下列其中一種:一有機電子元件,其包含:一有機發光二極體(OLED)、一聚合物發光二極體(PLED)、一光伏打、一超穎物質(metamaterial)、一薄膜電晶體;以及一波導;一無機電子元件,其包含:一發光二極體(LED)、一光伏打、一超穎物質、一薄膜電晶體;以及一波導;一光電元件,其包含:一光學開關;一波導;一可撓式基板;一食物容器;以及一藥品容器。
- 一種密閉性密封元件,其包含:一基板;至少一個有機組件;以及一經濺鍍密封材料,其中該至少一個組件係密閉性密封於該經濺鍍密封材料及該基板之間,其中在將該密封 材料濺鍍於該至少一個有機組件以及該基板上之前,該基板被冷卻至約<15℃的溫度,以及其中該經濺鍍材料為一低液相線溫度無機材料或一含Sn2+ 無機氧化物材料。
- 如申請專利範圍第22項之元件,其中該低液相線溫度無機材料為下列其中一項或其任何組合:錫-氟磷酸鹽材料;摻雜鎢之錫-氟磷酸鹽材料;硫屬化物材料;碲酸鹽材料;硼酸鹽材料;以及磷酸鹽材料。
- 如申請專利範圍第22項之元件,其中該含Sn2+ 無機氧化物材料為下列其中一項或其任何組合:SnO;SnO以及一硼酸鹽材料;SnO以及一磷酸鹽材料;以及SnO以及一硼磷酸鹽材料。
- 一種製造密閉性密封元件之方法,該方法包含下列步驟:冷卻一元件; 沉積一密封材料於該元件的至少一部份上;以及熱處理該元件以形成該密閉性密封元件,其中該密封材料為一低液相線溫度無機材料或一含Sn2+ 無機氧化物材料。
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- 2008-06-17 JP JP2010513230A patent/JP2010532070A/ja active Pending
- 2008-06-17 EP EP15180988.6A patent/EP2975664A1/en not_active Withdrawn
- 2008-06-17 EP EP08768546.7A patent/EP2054956B1/en not_active Expired - Fee Related
- 2008-06-17 CN CN2008800211113A patent/CN101689614B/zh not_active Expired - Fee Related
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Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
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TWI658621B (zh) * | 2013-07-12 | 2019-05-01 | 南韓商三星顯示器有限公司 | 有機發光顯示裝置 |
Also Published As
Publication number | Publication date |
---|---|
US20070252526A1 (en) | 2007-11-01 |
KR20100050470A (ko) | 2010-05-13 |
KR101265862B1 (ko) | 2013-05-20 |
US7722929B2 (en) | 2010-05-25 |
WO2008156762A1 (en) | 2008-12-24 |
CN101689614A (zh) | 2010-03-31 |
US8435604B2 (en) | 2013-05-07 |
CN101689614B (zh) | 2012-07-11 |
EP2975664A1 (en) | 2016-01-20 |
JP2010532070A (ja) | 2010-09-30 |
EP2054956A1 (en) | 2009-05-06 |
US20100193353A1 (en) | 2010-08-05 |
EP2054956B1 (en) | 2017-08-23 |
TW200919656A (en) | 2009-05-01 |
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