TW200537983A - Film-type getter and producing method thereof - Google Patents

Film-type getter and producing method thereof Download PDF

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TW200537983A
TW200537983A TW093112467A TW93112467A TW200537983A TW 200537983 A TW200537983 A TW 200537983A TW 093112467 A TW093112467 A TW 093112467A TW 93112467 A TW93112467 A TW 93112467A TW 200537983 A TW200537983 A TW 200537983A
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film
patent application
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group
item
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TW093112467A
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TWI257269B (en
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Byoung-Chul Lee
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Byoung-Chul Lee
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Priority to TW093112467A priority Critical patent/TWI257269B/en
Priority to PCT/KR2005/001304 priority patent/WO2005107334A1/en
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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
    • H05B33/02—Details
    • H05B33/04—Sealing arrangements, e.g. against humidity
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
    • B01D53/02—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by adsorption, e.g. preparative gas chromatography
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
    • B01J20/0203—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of metals not provided for in B01J20/04
    • B01J20/0225—Compounds of Fe, Ru, Os, Co, Rh, Ir, Ni, Pd, Pt
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
    • B01J20/0203—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of metals not provided for in B01J20/04
    • B01J20/024—Compounds of Zn, Cd, Hg
    • B01J20/0244—Compounds of Zn
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
    • B01J20/0203—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of metals not provided for in B01J20/04
    • B01J20/0248—Compounds of B, Al, Ga, In, Tl
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
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    • B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
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    • B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
    • B01J20/28002—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their physical properties
    • B01J20/28004—Sorbent size or size distribution, e.g. particle size
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
    • B01J20/28014—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their form
    • B01J20/2803—Sorbents comprising a binder, e.g. for forming aggregated, agglomerated or granulated products
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
    • B01J20/28014—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their form
    • B01J20/28033—Membrane, sheet, cloth, pad, lamellar or mat
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/30—Processes for preparing, regenerating, or reactivating
    • B01J20/3007—Moulding, shaping or extruding
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B13/00—Oxygen; Ozone; Oxides or hydroxides in general
    • C01B13/02—Preparation of oxygen
    • C01B13/0229—Purification or separation processes
    • C01B13/0248—Physical processing only
    • C01B13/0259—Physical processing only by adsorption on solids
    • C01B13/0281—Physical processing only by adsorption on solids in getters
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B3/00—Hydrogen; Gaseous mixtures containing hydrogen; Separation of hydrogen from mixtures containing it; Purification of hydrogen
    • C01B3/0005—Reversible uptake of hydrogen by an appropriate medium, i.e. based on physical or chemical sorption phenomena or on reversible chemical reactions, e.g. for hydrogen storage purposes ; Reversible gettering of hydrogen; Reversible uptake of hydrogen by electrodes
    • C01B3/001—Reversible uptake of hydrogen by an appropriate medium, i.e. based on physical or chemical sorption phenomena or on reversible chemical reactions, e.g. for hydrogen storage purposes ; Reversible gettering of hydrogen; Reversible uptake of hydrogen by electrodes characterised by the uptaking medium; Treatment thereof
    • C01B3/0026—Reversible uptake of hydrogen by an appropriate medium, i.e. based on physical or chemical sorption phenomena or on reversible chemical reactions, e.g. for hydrogen storage purposes ; Reversible gettering of hydrogen; Reversible uptake of hydrogen by electrodes characterised by the uptaking medium; Treatment thereof of one single metal or a rare earth metal; Treatment thereof
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B3/00—Hydrogen; Gaseous mixtures containing hydrogen; Separation of hydrogen from mixtures containing it; Purification of hydrogen
    • C01B3/0005—Reversible uptake of hydrogen by an appropriate medium, i.e. based on physical or chemical sorption phenomena or on reversible chemical reactions, e.g. for hydrogen storage purposes ; Reversible gettering of hydrogen; Reversible uptake of hydrogen by electrodes
    • C01B3/001—Reversible uptake of hydrogen by an appropriate medium, i.e. based on physical or chemical sorption phenomena or on reversible chemical reactions, e.g. for hydrogen storage purposes ; Reversible gettering of hydrogen; Reversible uptake of hydrogen by electrodes characterised by the uptaking medium; Treatment thereof
    • C01B3/0031—Intermetallic compounds; Metal alloys; Treatment thereof
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B3/00—Hydrogen; Gaseous mixtures containing hydrogen; Separation of hydrogen from mixtures containing it; Purification of hydrogen
    • C01B3/50—Separation of hydrogen or hydrogen containing gases from gaseous mixtures, e.g. purification
    • C01B3/508—Separation of hydrogen or hydrogen containing gases from gaseous mixtures, e.g. purification by selective and reversible uptake by an appropriate medium, i.e. the uptake being based on physical or chemical sorption phenomena or on reversible chemical reactions
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L23/00—Details of semiconductor or other solid state devices
    • H01L23/16—Fillings or auxiliary members in containers or encapsulations, e.g. centering rings
    • H01L23/18—Fillings characterised by the material, its physical or chemical properties, or its arrangement within the complete device
    • H01L23/26—Fillings characterised by the material, its physical or chemical properties, or its arrangement within the complete device including materials for absorbing or reacting with moisture or other undesired substances, e.g. getters
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2253/00—Adsorbents used in seperation treatment of gases and vapours
    • B01D2253/10—Inorganic adsorbents
    • B01D2253/112—Metals or metal compounds not provided for in B01D2253/104 or B01D2253/106
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2253/00—Adsorbents used in seperation treatment of gases and vapours
    • B01D2253/10—Inorganic adsorbents
    • B01D2253/112—Metals or metal compounds not provided for in B01D2253/104 or B01D2253/106
    • B01D2253/1126—Metal hydrides
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2257/00—Components to be removed
    • B01D2257/10—Single element gases other than halogens
    • B01D2257/104—Oxygen
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2257/00—Components to be removed
    • B01D2257/10—Single element gases other than halogens
    • B01D2257/108—Hydrogen
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2257/00—Components to be removed
    • B01D2257/80—Water
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L2224/00—Indexing scheme for arrangements for connecting or disconnecting semiconductor or solid-state bodies and methods related thereto as covered by H01L24/00
    • H01L2224/73—Means for bonding being of different types provided for in two or more of groups H01L2224/10, H01L2224/18, H01L2224/26, H01L2224/34, H01L2224/42, H01L2224/50, H01L2224/63, H01L2224/71
    • H01L2224/732—Location after the connecting process
    • H01L2224/73251—Location after the connecting process on different surfaces
    • H01L2224/73253—Bump and layer connectors
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L2924/00—Indexing scheme for arrangements or methods for connecting or disconnecting semiconductor or solid-state bodies as covered by H01L24/00
    • H01L2924/10—Details of semiconductor or other solid state devices to be connected
    • H01L2924/11—Device type
    • H01L2924/12—Passive devices, e.g. 2 terminal devices
    • H01L2924/1204—Optical Diode
    • H01L2924/12044—OLED
    • 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
    • H10K59/874—Passivation; Containers; Encapsulations including getter material or desiccant
    • 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
    • Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/30—Hydrogen technology
    • Y02E60/32—Hydrogen storage

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Analytical Chemistry (AREA)
  • Inorganic Chemistry (AREA)
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  • Condensed Matter Physics & Semiconductors (AREA)
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  • Microelectronics & Electronic Packaging (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
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  • Environmental & Geological Engineering (AREA)
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  • Electroluminescent Light Sources (AREA)
  • Solid-Sorbent Or Filter-Aiding Compositions (AREA)

Abstract

The present invention relates to a flexible film-type getter for removing moisture, oxygen and hydrogen together, which is used in organic electro-luminescence (EL) displays that are sealed within enclosures to avoid failure caused by moisture, oxygen and hydrogen, as well as a producing method thereof. This inventive film-type getter which is so flexible that it can be easily attached to the inside of organic electro-luminescence (EL) displays upon its use, comprises: a moisture-getting component that reacts with moisture to generate hydrogen; an oxygen-getting component that reacts with oxygen to form solid oxides; a hydrogen reactive substance that reacts with or absorbs hydrogen; a hydrogenation catalyst; and a polymer binder that forms into and maintains a flexible film.

Description

200537983 九、發明說明： 【發明所屬之技術領域】 本發明是有關於一種在被封於圍圈（enclosure)中以避 免因濕氣、氧氣與氫氣而導致故障之有機電激發光 (electroluminescence，EL)顯示器中用以去除濕氣、氧氣與 氫氣的可挽性薄膜型材料(film-type material)及其製造方 【先前技術】 在有機電激發光顯示器中，電子電路元件係形成於密 封盒(sealed case)中，且此密封盒之後會被一低濕氣水汽傳 送率(moisture vapor transmission rate)的黏性聚合物封入。 然而’如果不能去除在封入(encapsulation)與使用期間渗透 的濕氣與氧氣以及操作期間產生的氫氣，有機電激發光顯 示器的效能將會劣化或是增加其内部壓力。尤其，濕氣被 吸收在有機電激發光顯示器的裝置(fitting)上，以致於在封 入期間大量流入有機電激發光顯示器中。由於這個緣故， ，，在早期去除之。用於有機電激發光顯示器中的濕氣、 氧氣與氫氣吸氣器(getter)之功能是根據濕氣、氧氣與氫氣 的，，率與量以及在平衡(equilibrium)狀態下的濕氣、氧氣 與氣氣平衡濃度所決定。好的吸氣器是以較快速的去除率 與較低的平衡濃度為特色。 濕氣吸氣器的例子包括使用物理吸附作用的濕氣吸氣 材料二如秒膠(silica gel)以及使用化學反應者。物理吸附劑 具有局平衡濕氣濃度且高度依賴溫度 ，以致於假使溫度升 13644pif 200537983 南至恰好在一般插作溫度範圍中，物理吸附劑將再度釋放 濕氣。 因此，用化學反應去除濕氣的濕氣吸氣材料較為適 合，例如鹼金屬氧化物、鹼土族金屬氧化物、硫酸鹽、金 屬鹵化物、高氯酸鹽與五氧化磷。不過，如果將其製成薄 膜狀，則其濕氣去除率將變得過低。 在過去已經使用很久的一種用氧氣吸氣器去除氧氣的 方法中，在真空中高溫下蒸發金屬，再與氧氣反應形成金 屬氧化物，這些氧化物之後將被冷凝於一密封盒的内壁表 面上。另一種方法疋把金屬粉末置於密封盒中，以便與氧 氣慢慢反應。不過，前面在密封盒的内壁表面上使用金屬 蒸汽的方法有缺點，就是其需在高溫下處理，而且製程也 難以實施，所以這種方法的使用被限制在只能用於特殊應 用中。而後前面使用金屬粉末的方法則有難以拿動而使其 難以用於小尺寸元件的缺點。 ^ 在一種已知的使用氫氣吸氣器去除氫氣的方法中，氫 氣被一氧化催化劑氧化，以轉變成濕氣。另一種方法是用 催化劑活化氫氣，再將其加到具有雙鍵或三鍵的有機物 中，如 1，4-二苯基丁二烯(i，4_diphenyl butadiene)或聚丁二 稀(polybutadiene) 〇 而美國專利第4405487號揭露了一種濕氣吸氣器，係 藉由將一鋁或鋅粉末與濕氣反應並於有催化劑的存在下藉 由與一不飽和有機物如1，4-二苯基丁二烯的鍵結而去除^ 果的氫氣。同時，也揭露一種利用熱壓(h〇t pressing)製造 13644pif 7 200537983 顆粒狀(pellet)的這種濕氣吸氣器的方法。不過，這種濕氣 吸氣器及其製法具有可能會產生灰塵以及無法製成可繞性 薄膜的缺點，因而使用不便於使用。 另外，曰本專利公開號平成3(1991)-261091揭露—種 用於有機電激發光元件的濕氣吸氣器，其中有五氧化鱗粉 末置於一透氣容器（air-permeable container)中，之後放置於 一有機發光元件内。但是，因為濕氣吸氣器是粉末狀的， 所以不便於使用。此外，由於五氧化構粉末與濕氣間的反 應所產生的磷酸具有約41〜44°C的低溶點，所以磷酸甚至 會在普通操作溫度下從容器洩漏而污染電子電路元件。 依照用來製造用於封住的電子元件中的濕氣吸氣器之 方法，美國專利第5304419號揭露了一種混合一壓感黏著 劑(press sensitive adhesive)與乾燥劑(desiccant)的方法、美 國專利第5401536號揭露了一種混合聚合物與石夕酸|呂粉末 的方法以及美國專利第5591379號揭露了一種混合一透濕 氣黏結劑(binder)與一種如分子篩（Sieve)的乾燥劑的方 法。然而，在這些專利中所揭露的濕氣吸氣器具有低濕氣 吸收率(absorption rate)的缺點，因為濕氣藉由物理吸附作 用渗入黏結劑的分子層。其他缺點是在一般使用溫度範圍 下’前述濕氣吸氣器會再度釋放濕氣。 美國專利第5882761號揭露了一種方法，係藉由在有 機電激發光顯示器中使用粉末狀的金屬氧化物、金屬硫化 物、金屬_化物與金屬高氯酸鹽或是藉由氣相沈積、濺鑛 或旋塗於有機電激發光顯示器内面上鍍上前述金屬氧化 13644pif 8 200537983 物、金屬硫化物、金屬鹵化物與金屬高氣酸鹽，以從有機 電激發光顯示器去除濕氣。 美國專利第6226890號揭露了一種方法，係藉由將一 濕氣吸氣器貼在密封電子元件上，以從此密封電子元件中 去除濕氣，其中濕氣吸氣器包括具有高濕汽穿透率 (moisture vapor transmission rate，MVTR)的一聚合物與金 屬氧化物、硫化物、鹵化物或高氯酸鹽的一混合物(biend)。 而美國專利第6063307號揭露了 一種從密封空間中的 空氣去除氩氣的方法，係藉由使用一鈀催化劑的氫氣對聚 丁二烯之附加(addition)反應。美國專利第6203869號揭露 一種去除氳氣的方法，其中使用氧化鈀將氫氣轉變為濕 氣，而依次被吸附到一分子濾網上。然而，這種方法具有 一個問題，即為物理吸附劑的分子濾網可能會再度釋出濕 氣。 【發明内容】 本發明的目的就是在提供一種薄膜型吸氣器，以去除 濕氣、氧氣與虱氣’因其可撓性而易於貼附在有機電激發 光顯示器内侧使用，而同時去除濕氣、氧氣與氫氣。 本發明提出一種薄膜型吸氣器，以去除濕氣、氧氣與 氫氣，因其可撓性而使其易於貼附在有機電激發光顯示器 内侧使用。這種薄膜型吸氣器包括：與濕氣反應而產生氩 氣的一吸濕氣成分(moisture_getting component)、與氧氣反 應而形成固體氧化物的一吸氧氣成分（〇Xygen_getHng component)、用以與氫氣反應或吸收氫氣的一氫氣反應物 13644pif 9 200537983 (hydrogen reactive substance)、一氫化催化劑(hydrogenation catalyst)以及一聚合物黏結劑(p〇iymer binder)，用以形成於 一可撓性薄膜中並維持該可撓性薄膜。 在可撓性薄膜型吸氣器中，吸濕氣成分是一種可與濕 氣反應產生虱氣的材料。而一金屬、一氫化金屬或其合金 或混合物可用來作為這種吸濕氣成分。 釗述金屬之範例包含鐘、納、鉀、铷、铯、鈹、鎂、 詞、懿、鋇、銘、鋅、鐵、鎳。氫化金屬之範例包含氫化 納、氫化鉀、氫化鈣、氫化锶、氳化鋁、氫化鋰鋁、氫化 鈉鋁、氩化鉀鋁與氫化鈣鋁。 金屬與氫化金屬較佳係具有較小的粒徑，因為粒徑愈 大’濕氣去除率愈低。金屬與氫化金屬具有小於1〇() μιη 之粒徑，且較佳是小於10μπι。 而吸氧軋成分是一種可與氧氣反應形成固體氧化物的 材料。可用一金屬作為這種吸氧氣成分，或是用如吸濕氣 成分所選擇的相同金屬來作為這種吸濕氣成分。 金屬之範例包含鐘、納、钟、物、絶、皱、鎮、約、 锶、鋇、鋁、鋅、鐵、鎳、銅、銻與鉍作為吸氧氣成分。 金屬較佳係具有較小的粒徑，因為粒徑愈大，濕氣去 除率愈低。金屬具有小於1〇〇 μιη之粒徑，且較佳是小於 10 μιη 〇 氫氣反應物是一種可與氫氣鍵結的物質，及其範例包 括具有雙鍵或三鍵的一低分子量有機材料或聚合物、具有 腈鍵(nitrile bond)的一低分子量有機物或聚合物、具有^氧 13644pif 10 200537983 鍵的一低分子量有機物或聚合物、具有酮鍵的一低分子量 有機材料或聚合物以及藉由吸附進結構(texture)中具有鍵 結鼠氣特性的一金屬物。 氫化催化劑是一種促使氫氣反應物的氫化作用之材 料，其範例包括鈀、氧化鈀、鉑、铑、釕及其混合物或合 金0 作為聚合物黏結劑，可用具有良好加工性 (processibility)的一熱塑樹脂或反應可固化樹脂 (reaction_curable resin)，以及較佳是一種在由金屬或金屬 鹵化物與濕氣之間產生的一鹼性化合物下具有高化學穩定 性的樹脂。作為這種具高化學穩定性的聚合物黏結劑，可 使用如前述之聚合物以及用如氫氣反應物所選擇的相同的 聚合物。 熱塑樹脂的範例包含聚烯烴(polyolefin)、不飽和聚烯 烴、取代聚烯烴、取代不飽和聚烯烴及其它無規共聚物 (random copolymer)與塊狀共聚物(block copolymer)。同 時，聚合物可使用如聚二苯氧化物(P〇lyPhenylene oxide)、 聚二苯疏化物及聚醚颯(polyethersulfone)。 聚婦煙的範例包含聚乙烤、聚丙稀、聚丁婦、聚(4_ 甲基戊烯）。不飽和聚烯烴的範例包含聚丁二烯與聚異戊二 烯。取代聚烯烴的範例包含聚苯乙烯、聚氯乙烯、聚氟乙 烯、聚偏二氯乙烯、聚偏二氟乙烯、聚四氟乙烯與聚氯三 氣乙稀。取代不飽和聚稀煙的枕例包含聚氣丁 ^一稀。 反應可固化樹脂的範例包含聚烯烴、不飽和聚烯烴、 13644pif 11 200537983 取代聚烯烴、取代不飽和聚烯烴及其它無規共聚物或塊狀 共聚物，其附有可聚合端群(polymerizable end groups)。 可聚合端群的範例包含經由輻射能(radiation energy) 開始聚合之端群’和經由熱度(heat)開始聚合之端群。 本發明用以去除濕氣、氧氣與氫氣之吸氣器較佳係被 製造成薄膜狀，以便非常方便使用。這種薄膜型吸氣器的 製造方法包括以下步驟：互相混合前述成分，以及藉由擠 壓（extrusion)以及/或是壓延(caien(jering)形成混合物於一 薄膜中。如果需要的話，製造方法可另外加上製作薄膜膠 黏劑之任一面的步驟。 為讓本發明之上述和其他目的、特徵和優點能更明顯 易懂，下文特舉較佳實施例，並配合所附圖式，作詳細說 明如下。 【實施方式】 在此使用的「薄膜型」是一種普通的命名，是指形成 具有小厚度、包含具有平滑表面或由編織製備的。如果需 要的話’本發_以去除濕氣、氧氣與氫氣之吸氣器也可 含有顏料或填料。 圖1為本發明所提供之一種有機電激發光元件的示意 圖叫參照圖1，有機電激發光元件包括一含乾燥劑薄膜 有機電激發光層14。而保護層U與15係於組I成一圍 圈而圍圈被进封膠13封住。含乾燥劑薄膜1〇則是依昭 本發明的-種薄膜型吸氣器，因其可撓性而易於貼附在保、 13644pif 12 200537983 護層li内側。有機電激發光層14是位於保護層η的内面 上，而隔絕層12是在有機電激發光層14與含乾燥劑薄膜 10之間。 實例1〜2 在下面表一中所給的組成物之成分被互相混合，且藉 由熔態擠壓(melt-extrusion)以及壓延(calendering)步驟將混 合物製造成一可撓性薄膜型吸氣器，用以去除濕氣、氧氣 與氫氣。這種製造出的可撓性薄膜型吸氣器被測量其濕 氣、氧氣與氫氣的去除率。 在下面的實例1〜8中，製造出的可撓性薄膜型吸氣器 在20°C的溫度與50°/。的相對濕度(humidity)下被測量其最 初濕氣去除率，在20。(：與3%〇2和97°/c>Ar的混合氣體中 被測量其最初氧氣去除率以及也在2〇〇c與3%H2和97%Ar 的混合氣體中被測量其最初氫氣去除率。 表一 實例1 實例2 材料名稱 mg 材料名稱 mg 吸濕氣成分 氫化鈉(NaH) 10 氫化鈣(CaH2) 10 吸氧氣成分 鈣(Ca) 20 鋅(Zn) 30 氫化催化劑 鈀(Pd，5%)+活性瑞 7 鈀(Pd，5%)+活性碳 6 氫氣反應物 聚異戊二烯/聚笨 60 聚丁二烯/聚苯乙 60 乙烯共聚物 烯共聚物 (polyisoprene/ (polybutadiene/poly polystyrene) styrene) 聚合物黏結劑 乙烯/丙烯彈性艚 20 聚四氤乙烯/丙烯 20 膜厚 ΙΟΟμπι ΙΟΟμπι 13644pif 13 200537983 製造出的可撓性薄膜型吸氣器被測量其最初濕氣、氧 氣以及氫氣去除率，且測量結果顯示於下表二。 表二 實例1 實例2 濕氣去除率 2.7 mg/l〇 cm2-hr 1.8 mg/10 cm2-hr 氧氣去除率 0·1 mg/10 cm2.24hrs 0.1 mg/10 cm2-24hrs 氫氣去除率 1·0 mg/l〇 cm2 hr 0.6 mg/10 cm2-hr 實例3〜4 在下面表三中所給的組成物之成分被互相混合，且藉 由熔態擠壓以及壓延步驟將混合物製造成一可撓性薄膜型 吸氣器，用以去除濕氣、氧氣與氫氣。 表三 實例3 實例4 材料名稱 mg 材料名稱 mg 吸濕氣成分 mc^) 10 鋅(Zn) 30 吸氧氣成分 鋁(A—1) 10 鈉(Na) 10 氫化催化劑 鈀+氧化鈀 10 鈀(Pd，5%)+活性 碳 6 氫氣反應物 Zr+Ni 40 聚異戊二烯/聚苯 乙烯共聚物 60 聚合物黏結劑 聚異戊二烯/聚苯 乙烯共聚物 40 %(4_甲基戊烯） 20 膜厚 ΙΟΟμπι ΙΟΟμπι 製，，的可撓性薄膜型吸氣器被測量其最初濕氣、氧 氣以及氫氣去除率，且測量結果顯示於下表四。 13644pif 200537983 表四 實例3 實例4 濕氣去除率 5.2 mg/10 cm2-hr 4.5 mg/10 cm2-hr 氧氣去除率 0.6 mg/10 cm2-24hrs 0.3 mg/10 cm2-24hrs 氫氣去除率 1·2 mg/10 cm2.hr 1.8 mg/10 cm2-hr 實例S〜6 在下面表五中所給的組成物之成分被互相混合，且藉 由熔態擠壓以及壓延步驟將混合物製造成一可撓性薄膜型 吸氣器，用以去除濕氣、氧氣與氫氣。 表五 實例5 實例6 材料名稱 mg 材料名稱 mg 吸濕氣成分 氫化鈣(CaH2) 10 氫化鋰鋁(LiAlH4) —--- 5 吸氧氣成分 鈣(Ca) 20 銘(A1) 5 氫化催化劑 鈀（Pd，5%)+活 性碳 7 把+氧化1巴 10 氫氣反應物 聚丁二烯/聚苯 乙烯共聚物 60 Ti-Co 40 聚合物黏結 劑 聚丙烯 20 聚異戊二浠/聚苯乙 烯共聚物 40 膜厚 ΙΟΟμιη ΙΟΟμιη ^ 製造出的可撓性薄膜型吸氣器被測量其最初濕氣、氧 13644pif 15 200537983 氣以及氫氣去除率，且測量結果顯示於下表六。 表六 實例5 實例6 濕氣去除率 2.2 mg/10 cm2*hr 8.3 mg/10 cm2-hr 氧氣去除率 0.2 mg/10 cm2.24hrs 0.5 mg/10 cm2-24hrs 氫氣去除率 1.2 mg/10 cm2-hr 1.3 mg/10 cm2.hr 實例7〜8 在下面表七中所給的組成物之成分被互相混合，且藉 由熔態擠壓、壓延以及UV固化步驟將混合物製造成一可 撓性薄膜型吸氣器，用以去除濕氣、氧氣與氫氣。 表七 實例7 實例8 材料名稱 mg 材料名稱 mg 吸濕氣成分 氫化鈣(CaH2) 10 氫化鈉(NaH) 10 吸氧氣成分 鈣(Ca) 20 IS(A1) 10 氫化催化劑 鈀(Pd，5%)+活性 7 鈀(Pd，5%)+活性 7 碳 碳 氫氣反應物/聚 合物黏結劑 聚丁二婦丙稀酸 酉旨 80 聚丁二烯丙烯酸 酯 80 UV固化劑 —笨基乙二銅二 4 二苯基乙二酮二 4 甲基縮S同(benzil dimethyl ketal) 甲基縮酮 膜厚 ΙΟΟμπι ΙΟΟμιη 製造出的可撓性薄膜型吸氣器被測量其最初濕氣、氧 13644pif 200537983 氣以及氫氣去除率，且測量結果顯示於下表八。 表八 實例7 實例8 濕氣去除率 6.5 mg/10 cm2-hr 9.8 mg/10 cm2-hr 氧氣去除率 0.5 mg/10 cm2-24hrs 0.2 mg/10 cm2-24hrs 氫氣去除率 3.4 mg/10 cm2-hr 2.7 mg/10 cm2-hr 上面實例1〜8的結果顯現由本發明製備之用以去除濕 氣、氧氣與氫氣的可撓性薄膜型吸氣器可有效地同時去除 濕氣、氧氣與氫氣。 實例9 由實例1〜8所製造的每個用以去除濕氣、氧氣與氫氣 的可撓性薄膜型吸氣器被裝在一有機電激發光顯示器中， 以及測量其在有機電激發光顯示器的效能中之惡化（晝素 降低)上的預防效能。觀察到的結果顯示於下表九中。這種 測量是在有機電激發光顯示器於70〇C與85%的相對濕度 下才呆作300小時之後所實施的。 表九200537983 IX. Description of the invention: [Technical field to which the invention belongs] The present invention relates to an organic electroluminescence (EL) which is enclosed in an enclosure to avoid failure due to moisture, oxygen, and hydrogen. ) Removable film-type material used to remove moisture, oxygen and hydrogen in displays and its manufacturer [prior art] In organic electroluminescent displays, electronic circuit elements are formed in sealed boxes ( sealed case), and the sealed box will be sealed by a viscous polymer with a low moisture vapor transmission rate. However, if the moisture and oxygen that penetrated during encapsulation and use and the hydrogen gas generated during operation cannot be removed, the performance of the organic electroluminescent display will deteriorate or increase its internal pressure. In particular, moisture is absorbed in the fitting of the organic electroluminescent display so that a large amount of it flows into the organic electroluminescent display during sealing. For this reason,, was removed early. The function of the getter for moisture, oxygen and hydrogen in organic electroluminescent display is based on the humidity, oxygen and hydrogen, the rate and quantity, and the moisture and oxygen in the equilibrium state. Determined by gas-gas equilibrium concentration. Good aspirators are characterized by faster removal rates and lower equilibrium concentrations. Examples of the moisture getter include a moisture getter material using a physical adsorption effect such as a silica gel and a chemical reactant. The physical adsorbent has a local equilibrium moisture concentration and is highly temperature-dependent, so that if the temperature rises 13644pif 200537983 south to just in the general interpolated temperature range, the physical adsorbent will release moisture again. Therefore, moisture getter materials that use chemical reactions to remove moisture are more suitable, such as alkali metal oxides, alkaline earth metal oxides, sulfates, metal halides, perchlorates, and phosphorus pentoxide. However, if it is made into a thin film, its moisture removal rate becomes too low. In a method that has been used for a long time to remove oxygen with an oxygen aspirator, the metal is evaporated under high temperature in a vacuum, and then reacts with oxygen to form metal oxides, which are then condensed on the inner wall surface of a sealed box. . Another method is to place the metal powder in a sealed box to slowly react with oxygen. However, the previous method of using metal vapor on the inner wall surface of the sealed box has the disadvantage that it needs to be processed at high temperatures and the process is difficult to implement, so the use of this method is limited to special applications. However, the previous method using metal powder has the disadvantage that it is difficult to handle and it is difficult to use it for small-sized components. ^ In a known method of removing hydrogen using a hydrogen aspirator, the hydrogen is oxidized by an oxidation catalyst to convert it to moisture. Another method is to activate hydrogen with a catalyst and add it to an organic substance having a double or triple bond, such as 1,4-diphenyl butadiene or polybutadiene. U.S. Patent No. 4,405,487 discloses a moisture getter by reacting an aluminum or zinc powder with moisture and reacting with an unsaturated organic substance such as 1,4-diphenyl in the presence of a catalyst. Butadiene bonds to remove hydrogen. At the same time, a method for manufacturing 13644pif 7 200537983 pellets of this type of moisture getter by hot pressing is also disclosed. However, such a moisture getter and its manufacturing method have the disadvantages that dust may be generated and a rollable film cannot be made, and therefore it is not convenient to use. In addition, Japanese Patent Publication No. Heisei 3 (1991) -261091 discloses a moisture getter for an organic electroluminescent element, in which pentoxide scale powder is placed in an air-permeable container. It is then placed in an organic light emitting element. However, since the moisture getter is powdery, it is not convenient to use. In addition, since the phosphoric acid produced by the reaction between pentoxide powder and moisture has a low melting point of about 41 ~ 44 ° C, phosphoric acid may leak from the container even at ordinary operating temperatures and contaminate electronic circuit components. According to a method for manufacturing a moisture getter in a sealed electronic component, U.S. Patent No. 5,304,419 discloses a method of mixing a press sensitive adhesive and a desiccant. Patent No. 5401536 discloses a method for mixing a polymer with oxalic acid | Lu powder and U.S. Patent No. 5591379 discloses a method for mixing a moisture-permeable binder with a desiccant such as molecular sieve. . However, the moisture getters disclosed in these patents have the disadvantage of a low moisture absorption rate because moisture penetrates the molecular layer of the adhesive by the physical adsorption effect. Another disadvantage is that the aforementioned moisture aspirator will release moisture again under the general use temperature range. U.S. Patent No. 5,827,761 discloses a method by using powdered metal oxides, metal sulfides, metal compounds and metal perchlorates in organic electroluminescent displays, or by vapor deposition, sputtering The inner surface of the organic electroluminescent display is coated with minerals or spin-coated with the aforementioned metal oxide 13644pif 8 200537983, metal sulfide, metal halide and metal peroxyacid to remove moisture from the organic electroluminescent display. U.S. Patent No. 6,226,890 discloses a method for removing moisture from a sealed electronic component by attaching a moisture getter to the sealed electronic component, wherein the moisture getter includes a device having high moisture vapor transmission. A polymer (moisture vapor transmission rate, MVTR) is a biend of a polymer with a metal oxide, sulfide, halide, or perchlorate. U.S. Patent No. 6063307 discloses a method for removing argon from air in a sealed space by adding hydrogen to a polybutadiene using a palladium catalyst. U.S. Patent No. 6,203,869 discloses a method of removing radon gas in which hydrogen is converted to moisture using palladium oxide and sequentially adsorbed onto a molecular filter. However, this method has a problem that the molecular sieve, which is a physical adsorbent, may release moisture again. [Abstract] The purpose of the present invention is to provide a film-type getter to remove moisture, oxygen and lice. Because of its flexibility, it is easy to attach to the inside of an organic electroluminescent display and use it while removing moisture. Gas, oxygen and hydrogen. The present invention proposes a film-type getter to remove moisture, oxygen, and hydrogen. Due to its flexibility, it can be easily attached to the inside of an organic electroluminescent display for use. This film-type getter includes: a moisture_getting component that generates argon by reacting with moisture, an oxygen-absorbing component (〇Xygen_getHng component) that reacts with oxygen to form a solid oxide, and Hydrogen reacts or absorbs a hydrogen reactant 13644pif 9 200537983 (hydrogen reactive substance), a hydrogenation catalyst, and a polymer binder, which are formed in a flexible film and This flexible film is maintained. In the flexible film type inhaler, the moisture absorbing component is a material that reacts with moisture to generate lice. And a metal, a hydrogenated metal or an alloy or a mixture thereof can be used as this moisture absorption component. Examples of Zhao metal include bell, sodium, potassium, rubidium, cesium, beryllium, magnesium, word, rubidium, barium, inscription, zinc, iron, nickel. Examples of the metal hydride include sodium hydride, potassium hydride, calcium hydride, strontium hydride, aluminum halide, lithium aluminum hydride, sodium aluminum hydride, potassium aluminum hydride, and calcium aluminum hydride. Metals and hydrogenated metals preferably have smaller particle sizes because the larger the particle size, the lower the moisture removal rate. Metals and hydrogenated metals have a particle size of less than 10 (μm), and preferably less than 10 μm. The oxygen absorption rolling component is a material that can react with oxygen to form a solid oxide. A metal may be used as the oxygen absorbing component, or the same metal as the moisture absorbing component selected as the moisture absorbing component. Examples of metals include bells, nano, bells, objects, insulation, wrinkles, towns, about, strontium, barium, aluminum, zinc, iron, nickel, copper, antimony, and bismuth as oxygen-absorbing components. The metal preferably has a smaller particle size because the larger the particle size, the lower the moisture removal rate. Metals have a particle size of less than 100 μιη, and preferably less than 10 μιη. The hydrogen reactant is a substance that can bond with hydrogen, and examples thereof include a low molecular weight organic material or a polymer having a double or triple bond Substances, a low molecular weight organic substance or polymer having a nitrile bond, a low molecular weight organic substance or polymer having an oxygen 13644 pif 10 200537983 bond, a low molecular weight organic material or polymer having a ketone bond, and by adsorption A metal object in the texture that has the characteristics of bonding mouse gas. Hydrogenation catalyst is a material that promotes the hydrogenation of hydrogen reactants. Examples include palladium, palladium oxide, platinum, rhodium, ruthenium, and mixtures or alloys thereof. As a polymer binder, a heat with good processibility can be used. A plastic resin or a reaction curable resin, and preferably a resin having a high chemical stability under a basic compound generated between a metal or a metal halide and moisture. As such a polymer adhesive having high chemical stability, a polymer as described above and the same polymer selected using a reactant such as hydrogen can be used. Examples of thermoplastic resins include polyolefins, unsaturated polyolefins, substituted polyolefins, substituted unsaturated polyolefins, and other random copolymers and block copolymers. At the same time, polymers such as polyphenylene oxide, polydiphenylene oxide, and polyethersulfone can be used. Examples of Polyfoam include Polyethylene, Polypropylene, Polybutylene, Poly (4-methylpentene). Examples of unsaturated polyolefins include polybutadiene and polyisoprene. Examples of substituted polyolefins include polystyrene, polyvinyl chloride, polyvinyl fluoride, polyvinylidene chloride, polyvinylidene fluoride, polytetrafluoroethylene, and polyvinyl chloride. Examples of pillows that replace unsaturated polysmoke include polybutadiene. Examples of reactive curable resins include polyolefins, unsaturated polyolefins, 13644pif 11 200537983 substituted polyolefins, substituted unsaturated polyolefins, and other random copolymers or block copolymers with polymerizable end groups attached ). Examples of the polymerizable end group include an end group that starts polymerization via radiation energy 'and an end group that starts polymerization through heat. The getter for removing moisture, oxygen, and hydrogen according to the present invention is preferably manufactured in a thin film shape, so as to be very convenient to use. The manufacturing method of such a film-type getter includes the steps of mixing the aforementioned components with each other, and forming a mixture in a film by extrusion and / or caien (jering). If necessary, a manufacturing method Steps for making any side of the film adhesive may be additionally added. In order to make the above and other objects, features, and advantages of the present invention more comprehensible, the preferred embodiments are described below with the accompanying drawings to make The detailed description is as follows. [Embodiment] The "thin film type" used here is a common name, which refers to the formation of a small thickness, including a smooth surface or prepared by weaving. If necessary, '本 发 _ to remove moisture 2. The getter of oxygen and hydrogen may also contain pigments or fillers. Figure 1 is a schematic diagram of an organic electro-optical light-emitting element provided by the present invention. Refer to FIG. 1. The organic electro-optical light-emitting element includes a desiccant-containing thin film organic electro-excitation. The light layer 14. The protective layer U and 15 are in a circle formed by the group I and the circle is sealed by the sealant 13. The desiccant-containing film 10 is a film type according to the present invention. The aspirator is easy to be attached to the inner layer of the protective layer 13644pif 12 200537983 because of its flexibility. The organic electroluminescent layer 14 is located on the inner surface of the protective layer η, and the insulating layer 12 is an organic electroluminescent layer 14 and desiccant-containing film 10. Examples 1 to 2 The components of the composition given in Table 1 below were mixed with each other, and the mixture was melted through a melt-extrusion and calendering step. A flexible film-type getter was manufactured to remove moisture, oxygen, and hydrogen. The manufactured flexible film-type getter was measured for its removal rate of moisture, oxygen, and hydrogen. In Examples 1 to 8, the manufactured flexible film type getter was measured for its initial moisture removal rate at a temperature of 20 ° C and a relative humidity of 50 ° / ° C, at 20 ° (: and The initial oxygen removal rate was measured in a mixed gas of 3% 〇2 and 97 ° / c> Ar, and the initial hydrogen removal rate was also measured in a mixed gas of 200c with 3% H2 and 97% Ar. Table Example 1 Example 2 Material name mg Material name mg Hygroscopic component sodium hydride (NaH) 10 Hydrogen Calcium (CaH2) 10 Oxygen-absorbing component Calcium (Ca) 20 Zinc (Zn) 30 Hydrogenation catalyst Palladium (Pd, 5%) + Reactive 7 Palladium (Pd, 5%) + Activated carbon 6 Hydrogen reactant polyisoprene Olefin / polybenzyl 60 polybutadiene / polystyrene 60 ethylene copolymer olefin copolymer (polyisoprene / (polybutadiene / poly polystyrene) styrene) polymer binder ethylene / propylene elasticity 20 polytetramethylene ethylene / propylene 20 film thickness IOOμμι ΙΟΟμπι 13644pif 13 200537983 The flexible membrane-type aspirator manufactured was measured for its initial moisture, oxygen, and hydrogen removal rates, and the measurement results are shown in Table 2 below. Table 2 Example 1 Example 2 Moisture removal rate 2.7 mg / lcm2-hr 1.8 mg / 10 cm2-hr Oxygen removal rate 0.1 mg / 10 cm 2.24hrs 0.1 mg / 10 cm2-24hrs Hydrogen removal rate 1.0 mg / l〇cm2 hr 0.6 mg / 10 cm2-hr Examples 3 to 4 The components of the composition given in Table 3 below are mixed with each other, and the mixture is made into a flexible product through melt extrusion and calendering steps. Membrane type aspirator to remove moisture, oxygen and hydrogen. Table 3 Example 3 Example 4 Material name mg Material name mg Moisture absorption component mc ^) 10 Zinc (Zn) 30 Oxygen absorption component Aluminum (A-1) 10 Sodium (Na) 10 Hydrogenation catalyst Palladium + Palladium oxide 10 Palladium (Pd 5%) + activated carbon 6 hydrogen reactant Zr + Ni 40 polyisoprene / polystyrene copolymer 60 polymer binder polyisoprene / polystyrene copolymer 40% (4-methylpentane Ethylene) 20 flexible film type aspirator made of 100μm, 100μm, and its initial moisture, oxygen, and hydrogen removal rates were measured, and the measurement results are shown in Table 4 below. 13644pif 200537983 Table 4 Example 3 Example 4 Moisture removal rate 5.2 mg / 10 cm2-hr 4.5 mg / 10 cm2-hr Oxygen removal rate 0.6 mg / 10 cm2-24hrs 0.3 mg / 10 cm2-24hrs Hydrogen removal rate 1.2 mg / 10 cm2.hr 1.8 mg / 10 cm2-hr Example S ~ 6 The components of the composition given in Table 5 below are mixed with each other, and the mixture is made into a flexible film by melt extrusion and calendering steps. Type aspirator to remove moisture, oxygen and hydrogen. Table 5 Example 5 Example 6 Material name mg Material name mg Moisture absorption component calcium hydride (CaH2) 10 Lithium aluminum hydride (LiAlH4) ----- 5 Oxygen absorption component calcium (Ca) 20 Ming (A1) 5 Hydrogenation catalyst palladium ( Pd, 5%) + activated carbon 7 oxidized + 1 bar 10 hydrogen reactant polybutadiene / polystyrene copolymer 60 Ti-Co 40 polymer binder polypropylene 20 polyisoprene / polystyrene copolymerization Object 40 film thickness 100μιη ΙΟΟμιη ^ The manufactured flexible film type aspirator was measured for its initial moisture, oxygen 13644pif 15 200537983 gas, and hydrogen removal rate, and the measurement results are shown in Table VI below. Table 6 Example 5 Example 6 Moisture removal rate 2.2 mg / 10 cm2 * hr 8.3 mg / 10 cm2-hr Oxygen removal rate 0.2 mg / 10 cm2.24hrs 0.5 mg / 10 cm2-24hrs Hydrogen removal rate 1.2 mg / 10 cm2- hr 1.3 mg / 10 cm2.hr Examples 7 to 8 The components of the composition given in Table 7 below are mixed with each other, and the mixture is made into a flexible film type by melt extrusion, calendering and UV curing steps. Aspirator to remove moisture, oxygen and hydrogen. Table 7 Example 7 Example 8 Material name mg Material name mg Moisture absorption component calcium hydride (CaH2) 10 Sodium hydride (NaH) 10 Oxygen absorption component calcium (Ca) 20 IS (A1) 10 Hydrogenation catalyst palladium (Pd, 5%) + Active 7 Palladium (Pd, 5%) + Active 7 Carbon-Carbon Hydrogen Reactant / Polymer Binder Polybutadiene Acrylic Acid Purpose 80 Polybutadiene Acrylate 80 UV Curing Agent—Bentyl Ethyl Copper 4 benzil dimethyl ketal methyl benzil ketal methyl ketal film thickness 100 μm ΙΟΟμιη The flexible membrane type aspirator manufactured was measured for its initial humidity, oxygen 13644 pif 200537983 gas, and The hydrogen removal rate is shown in Table 8 below. Table 8 Example 7 Example 8 Moisture removal rate 6.5 mg / 10 cm2-hr 9.8 mg / 10 cm2-hr Oxygen removal rate 0.5 mg / 10 cm2-24hrs 0.2 mg / 10 cm2-24hrs Hydrogen removal rate 3.4 mg / 10 cm2- hr 2.7 mg / 10 cm2-hr The results of Examples 1 to 8 above show that the flexible film-type aspirator prepared by the present invention to remove moisture, oxygen, and hydrogen can effectively remove moisture, oxygen, and hydrogen simultaneously. Example 9 Each of the flexible film-type getters manufactured in Examples 1 to 8 to remove moisture, oxygen, and hydrogen was installed in an organic electroluminescent display, and measured in an organic electroluminescent display Prevention of deterioration (decreased daylight) in the effectiveness of The observed results are shown in Table IX below. This measurement was performed after the organic electroluminescent display was left at 300 ° C and 85% relative humidity for 300 hours. Table nine

前面表九的結果表明由本發明製備之用以去> 氧氣J氫氣的可撓㈣膜型吸氣器在有機餘發光=器 的效能中之惡化上有預防效能 13644pif 200537983 4上所述’本發供用以去除難、氧氣與 可撓性薄膜型吸氣器及其製造方法，這種薄膜型吸考 易於貼附在有機電激發光顯示器内側使用。 、ΰ 雖然本發明已以較佳實施例揭露如上，秋 =發明’任何熟習此技藝者，在不脫離;發;:::: =犯圍内’當可作些許之更動與潤飾，因此本發明之保護 範圍當視後附之申請專利範圍所界定者為準。 【圖式簡單說明】 圖1為本發明所提供之一種有機電激發光元件的示意 圖。 【主要元件符號說明】 10:含乾燥劑薄膜 11、15 :保護層 12 :隔絕層 13 :密封膠 14:有機電激發光層 13644pif 18The results in Table 9 above indicate that the flexible diaphragm-type getter prepared by the present invention to remove > oxygen J hydrogen has a preventive effect on the deterioration of the performance of the organic residual luminescence = 13364pif 200537983 4 The invention provides a thin film type getter for removing difficult, oxygen and flexible materials, and a manufacturing method thereof. This thin film type test is easy to be attached to the inside of an organic electroluminescent display and used. , Ϋ́ Although the present invention has been disclosed above in a preferred embodiment, autumn = invention 'anyone who is familiar with this skill, will not leave; hair; :::: = guilty inside' should be changed and retouched slightly, so this The scope of protection of the invention shall be determined by the scope of the attached patent application. [Brief description of the drawings] FIG. 1 is a schematic diagram of an organic electro-optical light-emitting element provided by the present invention. [Description of main component symbols] 10: Desiccant-containing film 11, 15: Protective layer 12: Insulating layer 13: Sealant 14: Organic electroluminescent layer 13644pif 18

Claims (1)

200537983 十、申請專利範圍： 1·一種薄膜型吸氣器，適於在一有機電激發光顯示器 中用來去除濕氣、氧氣與氫氣，該薄膜型吸氣器包括： 一吸濕氣成分，與濕氣反應而產生氫氣； 一吸氧氣成分，與氧氣反應而形成固體氧化物； 一氳氣反應物，用以吸收氫氣或與氫氣反應； 一氫化催化劑；以及 一聚合物黏結劑，形成於一可撓性薄膜中並維持該可 挽性薄膜。 2·如申請專利範圍第1項所述之薄膜型吸氣器，其中 該吸濕氣成分係選自包括一金屬、一氫化金屬及其合金或 混合物之族群。 3·如申請專利範圍第2項所述之薄膜型吸氣器，其中 該金屬係選自包括鐘、納、卸、鈒7、絶、皱、鎮、j弓、銷、 鋇、銘、鋅、鐵、鎳及其合金或混合物之族群。 4·如申請專利範圍第2項所述之薄膜型吸氣器，其中 該氫化金屬係選自包括氫化鈉、氫化鉀、氫化鈣、氫化銘、 虱化銘、氫化鐘銘、氫化納銘、氩化卸銘、氫化妈銘及其 合金或混合物之族群。 5·如申請專利範圍第2_4項其中一項所述之薄膜型吸 氣器，其中該金屬或該氫化金屬具有小於1〇〇 μπΐ2粒徑。 6. 如申請專利範圍第2-4項其中一項所述之薄膜型吸 氣器’其中該金屬或該氫化金屬具有小於10 μπι之粒徑。 7. 如申請專利範圍第1項所述之薄膜型吸氣器，其中 13644pif 19 200537983 該吸氧氣成分是一金屬。 8·如申請專利範圍第7項所述之薄膜型吸氣器，其中 该金屬係選自包括链、鈉、鉀、條、鉋、鈹、鎮、辦、叙 鋇、鋁、鋅、鐵、鎳、銅、銻、鉍及其合金或混合物 9·如申請專利範圍第7項所述之薄膜型吸氣器，其 該金屬粒徑小於1 〇〇 pm。 ^ 1〇.如申請專利範圍第7項所述之薄膜型吸氣器，其中 。亥金屬粒彳空小於1 〇 pm。 11.如申請專利範圍第丨項所述之薄膜型吸氣器，其中 該氫氣反應物係選自包括具有雙鍵或三鍵的一低分子^ 機材料或聚合物、具有腈鍵的—低分子量有機物或聚=物 之族群、具有環氧鍵的一低分子量有機物或聚合物、^ 酮鍵的一低分子量有機材料或聚合物及其混合物之族群。 斤I2.如申請專利範圍第1項所述之薄膜型吸氣器，、其中 該氫氣反應物係選自包括： 〃 1) 鈮、鈕、鈦、釩與锆； 2) 鈦的一合金或混合物以及一金屬，該金屬係選自包 括鋁、鈷、鉻、銅、鐵、鑭、錳、鎳、矽、錫、釔盥 族群； 3) 锆的一合金或混合物以及一金屬，該金屬係選自包 括鋁、#、鉻、銅、鐵、鑭、錳、鎳、矽、錫、釔與鍅之 族群；以及 ^ 4) 含1)、2)與3)的一混合物。 13644pif 20 200537983 13.如申請專利範圍第丨項所述之薄膜型吸氣器，其中 該氫氣反應物係選自包括： 1) 1巴、翻、铑、釕、氧化鈀及其合金或混合物；以及 2) —過渡金屬的一合金或混合物以及一金屬，該金屬 係選自包括把、始、鍺與釕之族群。 14·如申請專利範圍第丨項所述之薄膜型吸氣器，其中 該聚合物黏結劑是一熱塑樹脂。 15·如申請專利範圍第14項所述之薄膜型吸氣器，其 中該熱塑樹脂係選自包括一聚烯烴、一不飽和聚烯烴、取 代聚烯烴、取代不飽和聚烯烴及其它無規共聚物與塊狀共 聚物之族群。 16·如申請專利範圍第Μ項所述之薄膜型吸氣器，其 中該熱塑树月曰係選自包括聚二苯氧化物、聚二苯硫化物及 其混合物之族群。 17·如申請專利範圍第15項所述之薄膜型吸氣器，其 中該聚烯烴係選自包括聚乙烯、聚丙烯、聚丁烯、^聚(4'_ 曱基戊烯)及其混合物之族群。 18.如申請專利範圍第15項所述之薄膜型吸氣器，其 中該不飽和聚烯烴係選自包括聚丁二烯、聚異戊二婦及^ 混合物之族群。 ^ 19·如申請專利範圍第15項所述之薄膜型吸氣器，其 中遠取代聚烯煙係選自包括聚苯乙烯、聚氯乙埽、聚氣乙 稀、聚偏一氣乙烯、聚偏二氟乙埽、聚四氟乙稀、聚氣三 氟乙烯及其混合物之族群。 a — 13644pif 21 200537983 20·如申請專利範圍第15項所述之薄膜型吸氣器，其 中該取代不飽和聚烯烴是聚氯丁二烯。 21.如申請專利範圍第1項所述之薄膜型吸氣器，其中 該聚合物黏結劑是一可聚合樹脂(polymerizable resin)。 22·如申請專利範圍第21項所述之薄膜型吸氣器，其 中該可聚合樹脂之聚合是經由轄射能或熱度(heat)開始的。 23· —種薄膜型吸氣器的製造方法，該薄膜型吸氣器適 於在一有機電激發光顯示器中去除濕氣、氧氣與氫氣，該 製造方法，包括以下步驟： 互相混合一吸濕氣成分、一吸氧氣成分、一氫氣反應 物、一氫化催化劑與一聚合物黏結劑成一混合物； 融化該混合物；以及 藉由擠壓與壓延其中之一形成融化的該混合物於一薄 膜中。 13644pif 22200537983 10. Scope of patent application: 1. A thin film type getter suitable for removing moisture, oxygen and hydrogen in an organic electroluminescent display. The thin film type getter includes: a moisture absorbing component, and Moisture reacts to generate hydrogen; a component that absorbs oxygen and reacts with oxygen to form a solid oxide; a tritium reactant that absorbs or reacts with hydrogen; a hydrogenation catalyst; and a polymer binder that forms in a The flexible film is maintained in the flexible film. 2. The film-type getter according to item 1 of the scope of the patent application, wherein the moisture absorption component is selected from the group consisting of a metal, a hydrogenated metal, and an alloy or a mixture thereof. 3. The film-type aspirator according to item 2 of the scope of the patent application, wherein the metal is selected from the group consisting of bell, sodium, unloading, 鈒 7, insulation, wrinkle, town, bow, pin, barium, inscription, zinc , Iron, nickel and their alloys or mixtures. 4. The film-type aspirator according to item 2 of the scope of the patent application, wherein the hydrogenated metal is selected from the group consisting of sodium hydride, potassium hydride, calcium hydride, hydrogenation inscription, lice inscription, hydrogenation inscription, hydrogenation inscription, The group of argon unloading, hydrogenated moming and its alloys or mixtures. 5. The thin-film type getter according to one of the items 2 to 4 of the scope of patent application, wherein the metal or the hydrogenated metal has a particle size of less than 100 μπΐ2. 6. The thin-film type getter according to one of items 2-4 of the scope of the patent application, wherein the metal or the hydrogenated metal has a particle size of less than 10 μm. 7. The thin film type getter as described in the first item of the patent application scope, wherein 13644pif 19 200537983 is an oxygen absorbing component which is a metal. 8. The thin film type getter as described in item 7 of the scope of patent application, wherein the metal is selected from the group consisting of chain, sodium, potassium, strip, planer, beryllium, town, office, barium, aluminum, zinc, iron, Nickel, copper, antimony, bismuth, and alloys or mixtures thereof 9. The film-type getter described in item 7 of the scope of the patent application, wherein the metal particle size is less than 1000 pm. ^ 1 10. The film-type aspirator according to item 7 of the scope of patent application, wherein. The helium metal particles are emptied less than 10 pm. 11. The film-type getter according to item 丨 of the patent application scope, wherein the hydrogen reactant is selected from the group consisting of a low-molecular organic material or polymer having a double or triple bond, and a nitrile-low A group of molecular weight organics or polymers, a group of low molecular weight organics or polymers with epoxy bonds, a group of low molecular weight organic materials or polymers with ketone bonds, and mixtures thereof. I2. The thin film type getter as described in item 1 of the scope of patent application, wherein the hydrogen reactant is selected from the group consisting of: 〃 1) niobium, button, titanium, vanadium and zirconium; 2) an alloy of titanium or A mixture and a metal selected from the group consisting of aluminum, cobalt, chromium, copper, iron, lanthanum, manganese, nickel, silicon, tin, and yttrium; 3) an alloy or mixture of zirconium and a metal, the metal system Selected from the group consisting of aluminum, #, chromium, copper, iron, lanthanum, manganese, nickel, silicon, tin, yttrium, and thallium; and ^ 4) a mixture containing 1), 2), and 3). 13644pif 20 200537983 13. The thin film type getter as described in item 丨 of the patent application range, wherein the hydrogen reactant is selected from the group consisting of: 1) 1 bar, turn, rhodium, ruthenium, palladium oxide, and alloys or mixtures thereof; And 2)-an alloy or mixture of transition metals and a metal selected from the group consisting of barium, starting, germanium and ruthenium. 14. The film-type getter according to item 丨 of the patent application scope, wherein the polymer binder is a thermoplastic resin. 15. The film-type getter according to item 14 of the scope of the patent application, wherein the thermoplastic resin is selected from the group consisting of a polyolefin, an unsaturated polyolefin, a substituted polyolefin, a substituted unsaturated polyolefin, and other random Copolymers and block copolymers. 16. The film-type getter according to item M of the scope of the patent application, wherein the thermoplastic tree is selected from the group consisting of polydiphenyl oxide, polydiphenylsulfide, and mixtures thereof. 17. The film-type getter as described in item 15 of the scope of patent application, wherein the polyolefin is selected from the group consisting of polyethylene, polypropylene, polybutene, poly (4'_fluorenylpentene), and mixtures thereof Ethnic group. 18. The film-type getter according to item 15 of the scope of the patent application, wherein the unsaturated polyolefin is selected from the group consisting of polybutadiene, polyisoprene, and mixtures thereof. ^ 19. The thin film type inhaler as described in item 15 of the scope of patent application, wherein the far-replaced polyolefin smoke system is selected from the group consisting of polystyrene, polyvinyl chloride, polyacetylene, polyvinylidene, polyvinylidene Difluoroacetam, polytetrafluoroethylene, polytrifluoroethylene, and mixtures thereof. a — 13644pif 21 200537983 20 · The film-type getter described in item 15 of the scope of patent application, wherein the substituted unsaturated polyolefin is polychloroprene. 21. The film-type getter according to item 1 of the scope of patent application, wherein the polymer binder is a polymerizable resin. 22. The film-type getter according to item 21 of the scope of patent application, wherein the polymerization of the polymerizable resin is started by controlling radiation energy or heat. 23 · —A method of manufacturing a thin-film type getter, which is suitable for removing moisture, oxygen, and hydrogen in an organic electroluminescent display. The manufacturing method includes the following steps: mixing with each other and absorbing moisture A gas component, an oxygen absorbing component, a hydrogen reactant, a hydrogenation catalyst, and a polymer binder into a mixture; melting the mixture; and forming the molten mixture in a film by extrusion and calendering one of them. 13644pif 22
TW093112467A 2004-05-04 2004-05-04 Film-type getter and producing method thereof TWI257269B (en)

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ITMI20071148A1 (en) 2007-06-05 2008-12-06 Getters Spa RECHARGEABLE LITHIUM BATTERIES INCLUDING MEDIA IN THE FORM OF A MULTILAYER POLYMERIC SHEET FOR THE ABSORPTION OF HARMFUL SUBSTANCES
ITMI20071147A1 (en) 2007-06-05 2008-12-06 Getters Spa RECHARGEABLE LITHIUM BATTERIES INCLUDING VEHICLES FOR THE ABSORPTION OF HARMFUL SUBSTANCES
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ITMI20021201A1 (en) * 2002-06-03 2003-12-03 Getters Spa ASSEMBLED INCLUDING AT LEAST A SUPPORT WITH STORAGE OF GETTER MATERIAL FOR USE IN ELECTROLUMINESCENT BODY SCREENS
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CN104659060B (en) * 2013-11-25 2018-08-31 乐金显示有限公司 Array substrate and the method for manufacturing the array substrate

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