TW202020236A - 撓性器件用基板 - Google Patents

撓性器件用基板 Download PDF

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TW202020236A
TW202020236A TW108132362A TW108132362A TW202020236A TW 202020236 A TW202020236 A TW 202020236A TW 108132362 A TW108132362 A TW 108132362A TW 108132362 A TW108132362 A TW 108132362A TW 202020236 A TW202020236 A TW 202020236A
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Taiwan
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substrate
oxide film
glass
stainless steel
flexible device
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TW108132362A
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TWI808256B (zh
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南部光司
宮崎俊彥
升田裕久
下村洋司
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日商東洋製罐集團控股股份有限公司
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    • H—ELECTRICITY
    • H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
    • H10K77/00—Constructional details of devices covered by this subclass and not covered by groups H10K10/80, H10K30/80, H10K50/80 or H10K59/80
    • H10K77/10—Substrates, e.g. flexible substrates
    • H10K77/111—Flexible substrates
    • 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
    • C03C3/00—Glass compositions
    • C03C3/04—Glass compositions containing silica
    • C03C3/062—Glass compositions containing silica with less than 40% silica by weight
    • C03C3/064—Glass compositions containing silica with less than 40% silica by weight containing boron
    • C03C3/066—Glass compositions containing silica with less than 40% silica by weight containing boron containing zinc
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C3/00—Glass compositions
    • C03C3/12—Silica-free oxide glass compositions
    • C03C3/122—Silica-free oxide glass compositions containing oxides of As, Sb, Bi, Mo, W, V, Te as glass formers
    • 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
    • C03C3/00—Glass compositions
    • C03C3/12—Silica-free oxide glass compositions
    • C03C3/14—Silica-free oxide glass compositions containing boron
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C8/00—Enamels; Glazes; Fusion seal compositions being frit compositions having non-frit additions
    • C03C8/02—Frit compositions, i.e. in a powdered or comminuted form
    • C03C8/04—Frit compositions, i.e. in a powdered or comminuted form containing zinc
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C8/00—Enamels; Glazes; Fusion seal compositions being frit compositions having non-frit additions
    • C03C8/14—Glass frit mixtures having non-frit additions, e.g. opacifiers, colorants, mill-additions
    • C03C8/16—Glass frit mixtures having non-frit additions, e.g. opacifiers, colorants, mill-additions with vehicle or suspending agents, e.g. slip
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    • C23C24/08—Coating starting from inorganic powder by application of heat or pressure and heat
    • C—CHEMISTRY; METALLURGY
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    • 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
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C28/00—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D
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    • 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
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C28/00—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D
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    • 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
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C28/00—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D
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    • C23C28/32—Coatings combining at least one metallic layer and at least one inorganic non-metallic layer including at least one pure metallic layer
    • C23C28/321—Coatings combining at least one metallic layer and at least one inorganic non-metallic layer including at least one pure metallic layer with at least one metal alloy layer
    • 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
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
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    • 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
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C28/00—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D
    • C23C28/30—Coatings combining at least one metallic layer and at least one inorganic non-metallic layer
    • C23C28/32—Coatings combining at least one metallic layer and at least one inorganic non-metallic layer including at least one pure metallic layer
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    • C—CHEMISTRY; METALLURGY
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    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C28/00—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D
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    • C23C28/34—Coatings combining at least one metallic layer and at least one inorganic non-metallic layer including at least one inorganic non-metallic material layer, e.g. metal carbide, nitride, boride, silicide layer and their mixtures, enamels, phosphates and sulphates
    • C—CHEMISTRY; METALLURGY
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    • G09F—DISPLAYING; ADVERTISING; SIGNS; LABELS OR NAME-PLATES; SEALS
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    • G09F9/30—Indicating arrangements for variable information in which the information is built-up on a support by selection or combination of individual elements in which the desired character or characters are formed by combining individual elements
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    • H—ELECTRICITY
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    • H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
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    • Y10T428/12493—Composite; i.e., plural, adjacent, spatially distinct metal components [e.g., layers, joint, etc.]
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Abstract

本發明關於一種撓性器件用基板，其具有：不銹鋼基材、形成於該不銹鋼基材的表面上之氧化物膜、及具有電絕緣性的鉍系玻璃在該氧化物膜的表面上形成層狀而成的玻璃層。本發明的撓性器件用基板除了具有優異的耐銹蝕性、水分阻隔性、玻璃層之密接性、彎折耐性及玻璃層表面的表面平滑性之外，尚易於製造及品質管理等。

Description

撓性器件用基板
本發明關於撓性器件用基板，更具體地，關於耐銹蝕性、水分阻隔性、彎折耐性及絕緣層之密接性優異，可理想地使用於有機EL相關之用途的撓性器件用基板。
用於有機EL照明及有機EL顯示器、有機薄膜太陽能電池、IC印刷電路、電子紙等的撓性器件用基板，除了要求水分阻隔性及阻氣性等阻隔性之外，還要求平滑性及絕緣性，而且也要求使以曲面的形式使用之用途、卷對卷之生產成為可能所需的優異的可撓性(彎折耐性)。 下列專利文獻1提出了在塑膠薄膜基材上依序疊層透明導電層、有機發光介質層、陰極層並藉由黏接層疊層金屬箔而得之有機EL元件的構造，但該塑膠薄膜基材在水分阻隔性、耐熱性方面並非令人滿意。 另外，下列專利文獻2提出了在不銹鋼基材上設置由聚醯亞胺樹脂構成之平坦化層而得之撓性器件用基板，但聚醯亞胺樹脂的吸水性高，故在水分阻隔性方面仍無法令人滿意。 此外，下列專利文獻3提出了在不銹鋼基材上將二氧化矽系玻璃予以製膜而成之可撓性太陽能電池基板，但二氧化矽系玻璃的熱膨脹係數一般而言比不銹鋼小，對不銹鋼基材的密接性不足，且二氧化矽系玻璃有不耐彎折加工、衝撃的問題。
為了解決這樣的問題，本案發明人等提出了在金屬基材的表面上形成鎳鍍敷層，並於該鎳鍍敷層的表面上疊層具有電絕緣性的鉍系玻璃而成的撓性器件用金屬基板(專利文獻4)。 ［先前技術文獻］ ［專利文獻］
［專利文獻1］日本特開2004-171806號公報 ［專利文獻2］日本特開2011-97007號公報 ［專利文獻3］日本特開2006-80370號公報 ［專利文獻4］日本特開2014-107053號公報
［發明所欲解決之課題］
該撓性器件用金屬基板雖具有優異的水分阻隔性；且以與金屬基材間有優異密接性的鉍系玻璃疊層；亦具有優異的絕緣性及平坦性；也因輕量而具有可撓性，但煅燒後的玻璃層表面上，卻會有小突起及眼孔(eye hole)的情況發生，而如此微小的缺陷將損及玻璃層的平滑性。 另外，在使用沒有生銹疑慮的不銹鋼基材作為金屬基材時，由於不銹鋼基材與玻璃層之間沒有充分的密接性，故有諸如彎折耐性不佳，玻璃層破碎並剝離的問題。
為了解決這樣的問題，本案發明人等提出一種撓性器件用基板，其具有：不銹鋼基材、形成於該不銹鋼基材的表面上之鎳鍍敷層、及具有電絕緣性的鉍系玻璃在該鎳鍍敷層的表面上形成層狀而成的玻璃層(國際公開第2018/235759)。 該撓性器件用基板，因為使用不銹鋼基材而有效防止生銹的可能，且因為在不銹鋼基材表面上形成鎳鍍敷層，不銹鋼基材及玻璃層的密接性顯著地提升，又因為具有優異的彎折耐性，即使作為撓性器件用基板使用，也不會發生玻璃層的剝離等情況，具有充分的可撓性。
本案發明人等，關於該先申請案之發明，為了簡化製程、品質管理並降低製造成本而進一步地進行研究，結果發現即使不形成鎳鍍敷層，藉由在不銹鋼基材表面上形成具有特定之厚度及組成的氧化物膜，仍可得到與形成有鎳鍍敷層的情況一樣的玻璃層之密接性。 因此，本發明的目的係提供耐銹蝕性、水分阻隔性、玻璃層之密接性、彎折耐性及玻璃層表面的表面平滑性優異，且製造、品質管理等也容易的撓性器件用基板。 ［解決課題之手段］
根據本發明，提供一種撓性器件用基板，其具有：不銹鋼基材、形成於該不銹鋼基材的表面上之氧化物膜、及具有電絕緣性的鉍系玻璃在該氧化物膜的表面上形成層狀而成的玻璃層。 在本發明的撓性器件用基板中， 1.該氧化物膜的厚度宜為30nm以上； 2.該氧化物膜的厚度宜為80nm以上； 3.從該氧化物膜及該玻璃層之間的界面往該氧化物膜的厚度方向20nm處之鉻濃度宜為30atomic%以上； 4.從該氧化物膜及該玻璃層之間的界面往該氧化物膜的厚度方向20nm處之鉻濃度宜為50atomic%以上； 5.該鉍系玻璃宜含有Bi2 O3 、ZnO、B2 O3 。
又根據本發明，提供一種撓性器件用基板用基材，其由不銹鋼基材及形成於該不銹鋼基材的表面上之氧化物膜所構成，且該氧化物膜的厚度係為30nm以上。 在本發明的撓性器件用基板用基材中，該氧化物膜的厚度為80nm以上係特別理想。 ［發明之效果］
本發明的撓性器件用基板中，因為使用不銹鋼基材而有效防止生銹的可能，且因為在不銹鋼基材表面上形成特定的氧化物膜，不銹鋼基材與玻璃層的密接性顯著地提升，又因為具有優異的彎折耐性，即使作為撓性器件用基板使用，也不會發生玻璃層的剝離等情況，具有充分的可撓性。 又因為不需要在不銹鋼基材表面上形成鎳鍍敷層，所以製造步驟減少，而且在玻璃層形成之前的品質管理也變得容易，故生產性優異。 再者，因為有能以緻密結構完全防止水分通過的玻璃層，水分阻隔性亦為優秀，可有效地作為有機EL關聯用基板而使用。
(撓性器件用基板) 本發明的撓性器件用基板中，藉由在不銹鋼基材表面形成氧化物膜而成的撓性器件用基板用基材的該氧化物膜表面形成玻璃層，可使氧化物膜與玻璃反應而形成密接層，並顯著提高不銹鋼基材與玻璃層間的密接性。結果如前述一般，彎折耐性提高且不發生玻璃層的剝離，亦可對應於卷對卷之步驟。 據認為本發明的撓性器件用基板中，在不銹鋼基材上形成之氧化物膜中存在著高濃度的鉻，從而氧化物膜與玻璃會發生反應並形成密接層，使不銹鋼基材與玻璃層間的密接性提高。
圖1為顯示本發明之撓性器件用基板的範例之剖面結構之圖，整體以1顯示之撓性器件用基板具有：由不銹鋼基材10及形成於不銹鋼基材10的表面上之氧化物膜11所構成之撓性器件用基板用基材2、及具有電絕緣性的鉍系玻璃在撓性器件用基板用基材2的氧化物膜11的表面上形成層狀而成的玻璃層12。
［不銹鋼基材］ 作為用於本發明的撓性器件用基板之不銹鋼基材，可使用所有已習知的不銹鋼，但可特別適合地使用鐵氧體(ferrite)系不銹鋼。另外，宜使用熱膨脹係數在9.9×10-6 ～21×10-6 /℃之範圍內，尤其在10×10-6 ～14×10-6 /℃之範圍內者。 不銹鋼基材的厚度落在10～200μm之範圍內，尤其落在25～100μm之範圍內係較理想，藉此可獲得充分的可撓性。
［氧化物膜］ 在本發明的撓性器件用基板中，於不銹鋼基材表面上所形成的氧化物膜，係藉由將不銹鋼基材表面在大氣等含氧環境下煅燒而形成，由從不銹鋼基材擴散之鐵、鉻及其他添加元素的氧化物所形成。 亦即，在本發明的撓性器件用基板中，藉由在不銹鋼基材表面上形成氧化物膜，在使玻璃層與不銹鋼基材表面密接(相互擴散)的過程中，存在於玻璃層中的氧不會被奪走，又即便被奪走，其程度也很小，所以玻璃層中的氧並不會缺損。因此，在玻璃層與不銹鋼基材間的界面出現組成偏差的程度，比起未形成有氧化物膜的情況(亦即，未將不銹鋼基材表面在含氧環境下煅燒的情況)還來得小，有效抑制了密接性的降低。
此外，此氧化物膜如前述一般，從該氧化物膜及該玻璃層之間的界面往該氧化物膜的厚度方向20nm處之鉻濃度(令Cr及Fe的合計量為100時的Cr量)係為30atomic%以上，宜為50atomic%以上，更宜為70atomic%以上，更甚宜為80atomic以上之量，形成富含鉻的氧化物膜。 如此，藉由形成富含鉻的氧化物膜，玻璃層及不銹鋼基材間的密接性係顯著地提高。亦即，鉻氧化物係非常緻密，反觀鐵氧化物比起鉻氧化物來得脆弱。因此，藉由不銹鋼基材表面(包含氧化物膜)的鉻濃度提高，從而形成脆弱的鐵氧化物之機率會降低，並且不銹鋼基材與玻璃層間的密接性會得到改善。
在本發明中，期望氧化物膜厚度為30nm以上，宜為80nm以上，更宜為90nm以上，更甚宜為100nm以上。若氧化物膜之厚度比上述範圍更薄，則與落在上述範圍內的情況相比並無法得到充分的玻璃層之密接性，從後述實施例的結果得知，當以玻璃層作為外側並予以彎折時，有可能無法獲得充分的彎折耐性。 又，氧化物膜越厚，在氧化物膜中含有的鉻量也越多，因此不銹鋼基材與玻璃層間的密接性會提高，彎折耐性也會提高，但氧化物膜的厚度超過2000nm的話，則氧化物膜會脆化並且彎折耐性降低，所以氧化物膜的厚度在2000nm以下、特別是1500nm以下係為較理想的。
［玻璃層］ 本發明的撓性器件用基板，係在上述之氧化物膜上形成有由具有優異的水分阻隔性及與不銹鋼基材間的優異的密接性的鉍系玻璃所構成的玻璃層作為絕緣層。 作為本發明中的鉍系玻璃，可理想地使用含有Bi2 O3 、ZnO、B2 O3 之鉍系玻璃。亦即，除了含有作為主成分的Bi2 O3 ，亦含有ZnO及B2 O3 作為必須成分，而且這些成分在接近共晶點的組成範圍內，藉此可形成難以結晶化的玻璃網絡構造，與上述氧化物膜組合在一起，可提供能有效抑制玻璃表面上眼孔之發生的撓性器件用基板。
作為該鉍系玻璃，軟化點溫度為300～500℃且具有電絕緣性之鉍系玻璃較為理想，就玻璃組成而言，宜含有作為主成分(尤其70重量%以上)之Bi2 O3 ，並不限於此，但Bi2 O3 之含量為70～84重量%，ZnO之含量為10～12重量%，B2 O3 之含量為6～12重量%之鉍系無鉛玻璃係特別理想。這些成分在上述範圍內的話，可抑制玻璃層的結晶化，可有效地抑制眼孔的發生。
鉍系玻璃除了含有上述必須成分之外，宜進一步含有SiO2 及/或Al2 O3 並使SiO2 為0～2重量%、Al2 O3 為0～1重量%之量。藉由摻合該等之中的至少一成分，可提高水分阻隔性等並安定化玻璃層。 此外鉍系玻璃除了含有上述必須成分之外，宜更含有CuO及/或NiO，藉由摻合2重量%以下之CuO及/或2重量%以下之NiO，可提高玻璃的熔融性。 又鉍系玻璃除了上述必須成分之外，亦可以1.5重量%以下之量含有Y2 O3 、ZrO2 、La2 O3 、CeO2 、TiO2 、CoO、Fe2 O3 中的任一者，藉此可提高玻璃的耐久性、但這些成分的摻合量過多的話反而有可能使玻璃的耐久性降低。又，這些成分也可組合使用多種，但在該情況下，其合計量宜在1.5重量%以下。
在本發明中，期望玻璃層的厚度為2～45μm，宜為5～20μm，更宜為5～16μm之範圍內。若玻璃層厚度比上述範圍薄，則相較於落在上述範圍內的情況有可能無法確保充分的絕緣性，而且有可能無法使不銹鋼基材的凹凸充分地平滑化。另一方面，若比上述範圍厚，則相較於落在上述範圍內的情況會有可撓性不佳之疑慮。
(撓性器件用基板的製造方法) 本發明的撓性器件用基板可藉由包括下列步驟之製造方法製造：氧化物膜形成步驟即撓性器件用基板用基材的製造步驟，在不銹鋼基材之至少一表面上形成氧化物膜；及玻璃層形成步驟，在該氧化物膜上形成鉍系玻璃層。
［氧化物膜形成步驟］ 在本發明的撓性器件用基板及用於該基板的製造之撓性器件用基板用基材的製造方法之中，藉由將不銹鋼基材在含氧環境中予以煅燒，可在不銹鋼基材表面上形成氧化物膜。 煅燒條件，只要能形成該氧化物膜，並無特別限制，但期望煅燒溫度係在200～1300℃，宜為1000～1250℃，更宜為1000～1100℃之溫度。在比該範圍的煅燒溫度更低的情況下，與有在該範圍的情況相比之下，將不能有效率地形成氧化物膜；另一方面，在煅燒溫度高於上述範圍時，取決於不銹鋼基材的厚度，有時不銹鋼基材會有變形之虞。 煅燒時間，可根據含氧環境的氧濃度、及煅燒溫度適宜地變更，在大氣中於上述溫度範圍內煅燒的情況下，10～500秒間的煅燒係為合適的。 氧化物膜，如前所述一般，期望予以形成在30nm以上，較佳在80nm以上，且在2000nm以下，較佳在1500nm以下的範圍內。
［玻璃層形成步驟］ 接著，在氧化物膜上形成鉍系玻璃層。 玻璃層的形成步驟，雖不限於此順序，但大致來說可藉由將玻璃粉體與媒液(vehicle)混合、分散以製備玻璃糊劑，將此玻璃糊劑塗覆在氧化物膜上並予以乾燥，然後進行煅燒而形成。
>玻璃糊劑的製備> 玻璃糊劑係藉由將由上述鉍系玻璃構成之玻璃料(glass frit)經粉碎後得到之玻璃粉體與媒液混合、分散而獲得。 玻璃粉體係藉由將上述玻璃原料混合，在800～1200℃的溫度下加熱使其熔融，再急冷得到玻璃料之後，將其粉碎而獲得。關於粉碎方法，可列舉JET粉碎、快速研磨(rapid mill)粉碎、球磨粉碎等習知的方法。 若玻璃粉體之平均粒徑為20μm以下，較佳為1～10μm，更佳為1～5μm之範圍內的話，則就獲得平滑的玻璃表面之觀點係較理想，為了得到這樣微細的粉體，利用上述粉碎方法中的JET粉碎係較佳。
接著將得到的玻璃粉體與媒液混合、分散。 混合、分散的方法，可例示利用具備攪拌葉片之旋轉式混合機及珠磨機、塗料震盪機、輥磨機、瑪瑙研缽、超音波等所為之分散方法，宜利用珠磨機、塗料震盪機、輥磨機進行混合、分散較理想。 又，視需要，可根據習知的配方添加習知的增黏劑、分散劑等至玻璃糊劑中。
與玻璃粉體一起構成糊劑的媒液係用於調整糊劑的黏性，可將黏結劑溶解在溶劑中以製備。 玻璃糊劑係較理想地含有上述玻璃粉體30～80重量%、黏結劑0～10重量%(不包含0)、溶劑10～70重量%之量。玻璃粉體的量少於上述範圍時，糊劑黏度變低，難以形成所期望厚度之玻璃層；另一方面，玻璃粉體的量多於上述範圍時，玻璃糊劑黏度變得過高而塗覆性變差。又黏結劑的量少於上述範圍時，塗佈性變差；另一方面，黏結劑的量多於上述範圍時，有可能在煅燒後殘留未分解物。又溶劑的量少於上述範圍時，糊劑黏度變得過高而塗覆性變差；另一方面，溶劑的量多於上述範圍時，糊劑黏度變得過低，難以形成所期望厚度之玻璃層。
對於媒液，可使用已習知的溶劑系或水系的媒液，雖不受限於此，但可例如以下的黏結劑及溶劑。 黏結劑可例示：甲基纖維素、乙基纖維素、羧基甲基纖維素、氧基乙基纖維素、​苄基纖維素、丙基纖維素、硝基纖維素等纖維素系樹脂；將甲基丙烯酸甲酯、甲基丙烯酸乙酯、甲基丙烯酸丁酯、甲基丙烯酸2-羥乙酯、丙烯酸丁酯、丙烯酸2-羥基乙酯等丙烯酸系單體中的1種以上予以聚合而得之丙烯酸系樹脂等有機樹脂；聚碳酸伸丙酯等脂肪族聚烯烴系碳酸酯樹脂，但不限於此。 另外，溶劑可根據所使用之黏結劑適當選擇，纖維素系樹脂的情況，可使用水、萜品醇、丁基卡必醇乙酸酯、乙基卡必醇乙酸酯等溶劑；丙烯酸系樹脂的情況，可使用甲基乙基酮、萜品醇、丁基卡必醇乙酸酯、乙基卡必醇乙酸酯等溶劑；脂肪族聚烯烴系碳酸酯的情況，可使用碳酸伸丙酯、三乙酸甘油酯等溶劑，但不限於此。
>玻璃糊劑的塗佈、乾燥、煅燒> 將製得之玻璃糊劑，以相應於玻璃糊劑黏度的塗佈方法塗覆在氧化物膜上。就塗佈方法而言，例如可利用塗佈棒、模塗機、輥塗機、凹版塗佈機、網版印刷、平版(offset)印刷、塗抹器等進行塗覆，但不限於此。 經塗覆的玻璃糊劑在80～180℃的溫度進行乾燥。乾燥後，視需要進行脫膠(debinding)處理。脫膠處理宜在180～450℃的溫度加熱10分鐘以上。 乾燥後，將視需要予以脫膠處理後的塗佈面在550～900℃，較佳為650～900℃的溫度煅燒10～300秒，藉此形成玻璃層。煅燒溫度低於上述範圍時，相較於為上述範圍內的情形，會有熔融不充分之虞；另一方面，煅燒溫度高於上述範圍時，相較於為上述範圍內的情形，會有對玻璃表面造成影響之虞。
(有機EL器件用基板) 圖2為顯示使用了圖1所示之本發明的撓性器件用基板之有機EL器件用基板之範例之剖面結構的圖。 整體以1顯示之撓性器件用基板，係在兩面形成有氧化物膜11a、11b的不銹鋼基材10的一側之氧化物膜11a的表面上形成玻璃層12。 整體以3顯示之有機EL器件用基板，至少具有在該撓性器件用基板1的玻璃層12上形成之電極層(Ag、Al)20、在電極層20上形成之有機薄膜發光層21、在有機薄膜發光層21上形成之透明電極層22。圖2中顯示之具體例，係在透明電極層22上進一步疊層有透明密封層23、透明密封材24，並在氧化物膜11b上疊層有耐腐蝕性層25。
此外，雖未圖示，但亦可在圖2中所示之玻璃層12上形成對電極層具有優異密接性的基底層。 針對此種基底層，可藉由濺鍍法、蒸鍍法、CVD法等已習知的方法以形成鎳(Ni)、氧化銦錫(ITO)、銀(Ag)、金(Au)、銅(Cu)、鎂-銀(MgAg)、金-銅(AuCu)、銀-銅(AgCu)、氧化鋅(ZnO)、鈷(Co)、鈀(Pd)等金屬或金屬氧化物，尤其以濺鍍法進行成膜較為理想。 此基底層可對於在有機EL基板中所使用的由鋁(Al)、銀(Ag)、金(Au)及它們的合金等所構成之所有電極層展現出優異的密接性，尤其形成由鋁(Al)、銀(Ag)所構成之電極層時，基底層由上述金屬或金屬氧化物當中的鎳、氧化銦錫構成係較理想。 基底層的厚度宜在5～100nm的範圍內。 ［實施例］
1.不銹鋼基材 使用厚度0.05mm的以下4種材料作為不銹鋼基材。 SUS430MA：鐵氧體系不銹鋼箔(日本金屬(股)公司製) JFE443CT：鐵氧體系不銹鋼箔(JFE鋼鐵(股)公司製) NCA-1：鐵氧體系不銹鋼箔(日新製鋼(股)公司製) SUS430：鐵氧體系不銹鋼箔(日新製鋼(股)公司製)
2.煅燒處理(氧化物膜的形成) 以表2中所示條件，對不銹鋼基材表面實施20秒的熱處理。
3.玻璃層的形成 脫脂步驟：以浸過酒精的紗布擦拭各試樣之表面，進行脫脂。 塗膜形成步驟：準備混合有有機溶劑及黏結劑之媒液，利用研缽將媒液與表1記載之組成的鉍系玻璃粉體以使重量比成為25：75的方式予以混合，再以陶瓷製輥磨機進行分散處理，製得塗膜形成用玻璃糊劑。利用塗佈棒以使煅燒後的膜厚成為10μm的方式塗佈玻璃糊劑。之後，使用電氣爐進行乾燥(溫度：150℃、時間：3分鐘)、脫膠(溫度：330℃、時間：20分鐘)、煅燒(溫度：850℃、時間：30秒)，形成玻璃層。
［表1］
Figure 02_image001
4.評價 (1)氧化物膜的厚度 使用場發射歐傑電子能譜分析儀(AES：日本電子公司製，型號：JAMP-9500F)以測定由實施例及比較例得到的撓性器件用基板用基材的氧化物膜厚度。
(2)彎折耐性 將實施例及比較例中得到的撓性器件用基板以使玻璃層成為外側、或使玻璃層成為內側的方式分別予以捲繞在直徑(φ)為30mm、20mm、10mm的不銹鋼製圓棒，並以目視觀察是否發生剝離、裂紋。結果顯示在表2中。 另外，評價標準如下。 是否發生因捲繞測試所致之剝離、裂紋(目視觀察) ◎：無從玻璃/基材界面的剝離，無裂紋 ○：無從玻璃/基材界面的剝離，有裂紋(程度極小) △：無從玻璃/基材界面的剝離，有裂紋(程度小) ×：有從玻璃/基材界面的剝離，有裂紋
另外，綜合評價標準如下。 ◎：以玻璃層為外側進行捲繞時的φ20的評價為◎；且以玻璃層為內側進行捲繞時的所有評價均為◎ ○：以玻璃層為外側進行捲繞時的φ30的評價為◎且φ20的評價為○；且以玻璃層為內側進行捲繞時的所有評價均為◎ △：以玻璃層為外側進行捲繞時的φ30的評價為◎且φ20的評價為△；且以玻璃層為內側進行捲繞時的所有評價均為◎ △△：以玻璃層為外側進行捲繞時的φ30的評價為○或△；且以玻璃層為內側進行捲繞時的所有評價均為◎ △△△：以玻璃層為外側進行捲繞時的所有評價為×；且以玻璃層為內側進行捲繞時的φ30及φ20為◎或所有評價均為◎ ×：以玻璃層為外側進行捲繞時的所有評價為×；且以玻璃層為內側進行捲繞時僅φ30的評價為◎
(3)鉻濃度(縱深分析) 針對由實施例2，4，9～14，21，24，25，27及比較例1～4獲得之撓性器件用基板用基材，藉由X射線光電子能譜分析(XPS)來測定從玻璃層及氧化物膜之間的界面往氧化物膜的厚度方向20nm處之鉻(Cr)量、及鐵(Fe)量，並由下列算式算出鉻濃度。結果顯示在表2中。 Cr濃度(atomic%)＝Cr/(Cr＋Fe)×100
［表2］
Figure 108132362-A0304-0001
 ［產業上可利用性］
本發明的撓性器件用基板具有優異的耐銹蝕性、水分阻隔性、絕緣性、彎折耐性、玻璃層的表面平滑性及密接性，可理想地作為有機EL照明、有機EL顯示器、有機薄膜太陽能電池、IC印刷電路、電子紙等的基板而使用。
1:撓性器件用基板 2:撓性器件用基板用基材 3:有機EL器件用基板 10:不銹鋼基材 11:氧化物膜 11a:氧化物膜 11b:氧化物膜 12:玻璃層 20:電極層(Ag、Al) 21:有機薄膜發光層 22:透明電極層 23:透明密封層 24:透明密封材 25:耐腐蝕性層
［圖1］為顯示本發明的撓性器件用基板之範例之剖面結構之圖。 ［圖2］為顯示使用了圖1所示之本發明的撓性器件用基板之有機EL器件用基板之剖面結構之圖。

Claims (8)

  1. 一種撓性器件用基板，其具有：不銹鋼基材、形成於該不銹鋼基材的表面上之氧化物膜、及具有電絕緣性的鉍系玻璃在該氧化物膜的表面上形成層狀而成的玻璃層。
  2. 如申請專利範圍第1項之撓性器件用基板，其中該氧化物膜的厚度係為30nm以上。
  3. 如申請專利範圍第1項之撓性器件用基板，其中該氧化物膜的厚度係為80nm以上。
  4. 如申請專利範圍第1至3項中任一項之撓性器件用基板，其中，從該氧化物膜及該玻璃層之間的界面往該氧化物膜的厚度方向20nm處之鉻濃度係為30atomic%。
  5. 如申請專利範圍第1至3項中任一項之撓性器件用基板，其中，從該氧化物膜及該玻璃層之間的界面往該氧化物膜的厚度方向20nm處之鉻濃度係為50atomic%。
  6. 如申請專利範圍第1至5項中任一項之撓性器件用基板，其中，該鉍系玻璃含有Bi2 O3 、ZnO、B2 O3 。
  7. 一種撓性器件用基板用基材，其由不銹鋼基材及形成於該不銹鋼基材的表面上之氧化物膜所構成，且該氧化物膜的厚度係為30nm以上。
  8. 如申請專利範圍第7項之撓性器件用基板用基材，其中，該氧化物膜的厚度係為80nm以上。
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