CN104589736A - 透明基板的制造方法 - Google Patents

透明基板的制造方法 Download PDF

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Publication number
CN104589736A
CN104589736A CN201410746255.2A CN201410746255A CN104589736A CN 104589736 A CN104589736 A CN 104589736A CN 201410746255 A CN201410746255 A CN 201410746255A CN 104589736 A CN104589736 A CN 104589736A
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CN
China
Prior art keywords
mentioned
thermoplastic resin
solvent
coating layer
unorganic glass
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Pending
Application number
CN201410746255.2A
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English (en)
Inventor
服部大辅
村重毅
龟山忠幸
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Nitto Denko Corp
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Nitto Denko Corp
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Publication date
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Publication of CN104589736A publication Critical patent/CN104589736A/zh
Pending legal-status Critical Current

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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C65/00—Joining or sealing of preformed parts, e.g. welding of plastics materials; Apparatus therefor
    • B29C65/48—Joining or sealing of preformed parts, e.g. welding of plastics materials; Apparatus therefor using adhesives, i.e. using supplementary joining material; solvent bonding
    • B29C65/4805—Joining or sealing of preformed parts, e.g. welding of plastics materials; Apparatus therefor using adhesives, i.e. using supplementary joining material; solvent bonding characterised by the type of adhesives
    • B29C65/481—Non-reactive adhesives, e.g. physically hardening adhesives
    • B29C65/482—Drying adhesives, e.g. solvent based adhesives
    • 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
    • C03C17/00—Surface treatment of glass, not in the form of fibres or filaments, by coating
    • C03C17/28—Surface treatment of glass, not in the form of fibres or filaments, by coating with organic material
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B17/00—Layered products essentially comprising sheet glass, or glass, slag, or like fibres
    • B32B17/06—Layered products essentially comprising sheet glass, or glass, slag, or like fibres comprising glass as the main or only constituent of a layer, next to another layer of a specific material
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C65/00—Joining or sealing of preformed parts, e.g. welding of plastics materials; Apparatus therefor
    • B29C65/48—Joining or sealing of preformed parts, e.g. welding of plastics materials; Apparatus therefor using adhesives, i.e. using supplementary joining material; solvent bonding
    • B29C65/52—Joining or sealing of preformed parts, e.g. welding of plastics materials; Apparatus therefor using adhesives, i.e. using supplementary joining material; solvent bonding characterised by the way of applying the adhesive
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C66/00—General aspects of processes or apparatus for joining preformed parts
    • B29C66/01—General aspects dealing with the joint area or with the area to be joined
    • B29C66/05—Particular design of joint configurations
    • B29C66/10—Particular design of joint configurations particular design of the joint cross-sections
    • B29C66/11—Joint cross-sections comprising a single joint-segment, i.e. one of the parts to be joined comprising a single joint-segment in the joint cross-section
    • B29C66/112—Single lapped joints
    • B29C66/1122—Single lap to lap joints, i.e. overlap joints
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C66/00—General aspects of processes or apparatus for joining preformed parts
    • B29C66/40—General aspects of joining substantially flat articles, e.g. plates, sheets or web-like materials; Making flat seams in tubular or hollow articles; Joining single elements to substantially flat surfaces
    • B29C66/41—Joining substantially flat articles ; Making flat seams in tubular or hollow articles
    • B29C66/45—Joining of substantially the whole surface of the articles
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C66/00—General aspects of processes or apparatus for joining preformed parts
    • B29C66/70—General aspects of processes or apparatus for joining preformed parts characterised by the composition, physical properties or the structure of the material of the parts to be joined; Joining with non-plastics material
    • B29C66/73—General aspects of processes or apparatus for joining preformed parts characterised by the composition, physical properties or the structure of the material of the parts to be joined; Joining with non-plastics material characterised by the intensive physical properties of the material of the parts to be joined, by the optical properties of the material of the parts to be joined, by the extensive physical properties of the parts to be joined, by the state of the material of the parts to be joined or by the material of the parts to be joined being a thermoplastic or a thermoset
    • B29C66/731—General aspects of processes or apparatus for joining preformed parts characterised by the composition, physical properties or the structure of the material of the parts to be joined; Joining with non-plastics material characterised by the intensive physical properties of the material of the parts to be joined, by the optical properties of the material of the parts to be joined, by the extensive physical properties of the parts to be joined, by the state of the material of the parts to be joined or by the material of the parts to be joined being a thermoplastic or a thermoset characterised by the intensive physical properties of the material of the parts to be joined
    • B29C66/7311—Thermal properties
    • B29C66/73117—Tg, i.e. glass transition temperature
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C66/00—General aspects of processes or apparatus for joining preformed parts
    • B29C66/70—General aspects of processes or apparatus for joining preformed parts characterised by the composition, physical properties or the structure of the material of the parts to be joined; Joining with non-plastics material
    • B29C66/73—General aspects of processes or apparatus for joining preformed parts characterised by the composition, physical properties or the structure of the material of the parts to be joined; Joining with non-plastics material characterised by the intensive physical properties of the material of the parts to be joined, by the optical properties of the material of the parts to be joined, by the extensive physical properties of the parts to be joined, by the state of the material of the parts to be joined or by the material of the parts to be joined being a thermoplastic or a thermoset
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    • B29C66/7318—Permeability to gases or liquids
    • B29C66/73181—Permeability to gases or liquids permeable
    • B29C66/73183—Permeability to gases or liquids permeable to liquids
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C66/00—General aspects of processes or apparatus for joining preformed parts
    • B29C66/70—General aspects of processes or apparatus for joining preformed parts characterised by the composition, physical properties or the structure of the material of the parts to be joined; Joining with non-plastics material
    • B29C66/73—General aspects of processes or apparatus for joining preformed parts characterised by the composition, physical properties or the structure of the material of the parts to be joined; Joining with non-plastics material characterised by the intensive physical properties of the material of the parts to be joined, by the optical properties of the material of the parts to be joined, by the extensive physical properties of the parts to be joined, by the state of the material of the parts to be joined or by the material of the parts to be joined being a thermoplastic or a thermoset
    • B29C66/733—General aspects of processes or apparatus for joining preformed parts characterised by the composition, physical properties or the structure of the material of the parts to be joined; Joining with non-plastics material characterised by the intensive physical properties of the material of the parts to be joined, by the optical properties of the material of the parts to be joined, by the extensive physical properties of the parts to be joined, by the state of the material of the parts to be joined or by the material of the parts to be joined being a thermoplastic or a thermoset characterised by the optical properties of the material of the parts to be joined, e.g. fluorescence, phosphorescence
    • B29C66/7336—General aspects of processes or apparatus for joining preformed parts characterised by the composition, physical properties or the structure of the material of the parts to be joined; Joining with non-plastics material characterised by the intensive physical properties of the material of the parts to be joined, by the optical properties of the material of the parts to be joined, by the extensive physical properties of the parts to be joined, by the state of the material of the parts to be joined or by the material of the parts to be joined being a thermoplastic or a thermoset characterised by the optical properties of the material of the parts to be joined, e.g. fluorescence, phosphorescence at least one of the parts to be joined being opaque, transparent or translucent to visible light
    • B29C66/73365—General aspects of processes or apparatus for joining preformed parts characterised by the composition, physical properties or the structure of the material of the parts to be joined; Joining with non-plastics material characterised by the intensive physical properties of the material of the parts to be joined, by the optical properties of the material of the parts to be joined, by the extensive physical properties of the parts to be joined, by the state of the material of the parts to be joined or by the material of the parts to be joined being a thermoplastic or a thermoset characterised by the optical properties of the material of the parts to be joined, e.g. fluorescence, phosphorescence at least one of the parts to be joined being opaque, transparent or translucent to visible light at least one of the parts to be joined being transparent or translucent to visible light
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C66/00—General aspects of processes or apparatus for joining preformed parts
    • B29C66/70—General aspects of processes or apparatus for joining preformed parts characterised by the composition, physical properties or the structure of the material of the parts to be joined; Joining with non-plastics material
    • B29C66/73—General aspects of processes or apparatus for joining preformed parts characterised by the composition, physical properties or the structure of the material of the parts to be joined; Joining with non-plastics material characterised by the intensive physical properties of the material of the parts to be joined, by the optical properties of the material of the parts to be joined, by the extensive physical properties of the parts to be joined, by the state of the material of the parts to be joined or by the material of the parts to be joined being a thermoplastic or a thermoset
    • B29C66/735—General aspects of processes or apparatus for joining preformed parts characterised by the composition, physical properties or the structure of the material of the parts to be joined; Joining with non-plastics material characterised by the intensive physical properties of the material of the parts to be joined, by the optical properties of the material of the parts to be joined, by the extensive physical properties of the parts to be joined, by the state of the material of the parts to be joined or by the material of the parts to be joined being a thermoplastic or a thermoset characterised by the extensive physical properties of the parts to be joined
    • B29C66/7352—Thickness, e.g. very thin
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C66/00—General aspects of processes or apparatus for joining preformed parts
    • B29C66/70—General aspects of processes or apparatus for joining preformed parts characterised by the composition, physical properties or the structure of the material of the parts to be joined; Joining with non-plastics material
    • B29C66/73—General aspects of processes or apparatus for joining preformed parts characterised by the composition, physical properties or the structure of the material of the parts to be joined; Joining with non-plastics material characterised by the intensive physical properties of the material of the parts to be joined, by the optical properties of the material of the parts to be joined, by the extensive physical properties of the parts to be joined, by the state of the material of the parts to be joined or by the material of the parts to be joined being a thermoplastic or a thermoset
    • B29C66/739—General aspects of processes or apparatus for joining preformed parts characterised by the composition, physical properties or the structure of the material of the parts to be joined; Joining with non-plastics material characterised by the intensive physical properties of the material of the parts to be joined, by the optical properties of the material of the parts to be joined, by the extensive physical properties of the parts to be joined, by the state of the material of the parts to be joined or by the material of the parts to be joined being a thermoplastic or a thermoset characterised by the material of the parts to be joined being a thermoplastic or a thermoset
    • B29C66/7392—General aspects of processes or apparatus for joining preformed parts characterised by the composition, physical properties or the structure of the material of the parts to be joined; Joining with non-plastics material characterised by the intensive physical properties of the material of the parts to be joined, by the optical properties of the material of the parts to be joined, by the extensive physical properties of the parts to be joined, by the state of the material of the parts to be joined or by the material of the parts to be joined being a thermoplastic or a thermoset characterised by the material of the parts to be joined being a thermoplastic or a thermoset characterised by the material of at least one of the parts being a thermoplastic
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C66/00—General aspects of processes or apparatus for joining preformed parts
    • B29C66/70—General aspects of processes or apparatus for joining preformed parts characterised by the composition, physical properties or the structure of the material of the parts to be joined; Joining with non-plastics material
    • B29C66/74—Joining plastics material to non-plastics material
    • B29C66/746—Joining plastics material to non-plastics material to inorganic materials not provided for in groups B29C66/742 - B29C66/744
    • B29C66/7465—Glass
    • B—PERFORMING OPERATIONS; TRANSPORTING
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    • B29C66/83—General aspects of machine operations or constructions and parts thereof characterised by the movement of the joining or pressing tools
    • B29C66/834—General aspects of machine operations or constructions and parts thereof characterised by the movement of the joining or pressing tools moving with the parts to be joined
    • B29C66/8341—Roller, cylinder or drum types; Band or belt types; Ball types
    • B29C66/83421—Roller, cylinder or drum types; Band or belt types; Ball types band or belt types
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
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    • B29C66/00—General aspects of processes or apparatus for joining preformed parts
    • B29C66/80—General aspects of machine operations or constructions and parts thereof
    • B29C66/83—General aspects of machine operations or constructions and parts thereof characterised by the movement of the joining or pressing tools
    • B29C66/834—General aspects of machine operations or constructions and parts thereof characterised by the movement of the joining or pressing tools moving with the parts to be joined
    • B29C66/8341—Roller, cylinder or drum types; Band or belt types; Ball types
    • B29C66/83421—Roller, cylinder or drum types; Band or belt types; Ball types band or belt types
    • B29C66/83423—Roller, cylinder or drum types; Band or belt types; Ball types band or belt types cooperating bands or belts
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C66/00—General aspects of processes or apparatus for joining preformed parts
    • B29C66/90—Measuring or controlling the joining process
    • B29C66/91—Measuring or controlling the joining process by measuring or controlling the temperature, the heat or the thermal flux
    • B29C66/914—Measuring or controlling the joining process by measuring or controlling the temperature, the heat or the thermal flux by controlling or regulating the temperature, the heat or the thermal flux
    • B29C66/9141—Measuring or controlling the joining process by measuring or controlling the temperature, the heat or the thermal flux by controlling or regulating the temperature, the heat or the thermal flux by controlling or regulating the temperature
    • B29C66/91431—Measuring or controlling the joining process by measuring or controlling the temperature, the heat or the thermal flux by controlling or regulating the temperature, the heat or the thermal flux by controlling or regulating the temperature the temperature being kept constant over time
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    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
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    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
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Abstract

本发明提供一种弯曲性、挠性、耐冲击性以及外观优异的透明基板的制造方法。本发明的透明基板的制造方法包含：工序A，在具有溶剂透过性的支撑基材上涂布热塑性树脂(A)组合物溶液，形成涂布层；工序B，将无机玻璃的至少一个面与该涂布层经由粘接剂组合物贴合，形成层叠体；工序C，对该层叠体实施第1热处理，使该涂布层中的残留溶剂量减少至规定量；和，工序D，将该支撑基材从该层叠体上剥离后，进行第2热处理，使该涂布层干燥，形成热塑性树脂层。

Description

透明基板的制造方法
本申请是申请日为2011年4月28日、中国专利申请号为201180021854.2、发明名称为“透明基板的制造方法”(PCT/JP2011/060367号国际申请进入中国国家阶段)的发明专利的分案申请。
技术领域
本发明涉及一种透明基板的制造方法。
背景技术
近年来，由于影像通信技术的发展，如平面显示器(FPD；例如液晶显示装置、有机EL显示装置)这样的显示装置以及太阳电池不断推进轻量、薄型化。以往，对于显示装置以及太阳电池中使用的基板，在多数情况下使用玻璃基板。玻璃基板的透明性或耐溶剂性、阻气性、耐热性优异。但是，当谋求构成玻璃基板的玻璃的薄型化时，虽然在轻量化的同时挠性也优异，但产生如下的问题：耐冲击性变得不充分，操作变困难。
为了使薄型玻璃基板的操作性提高，提出了：在玻璃表面涂布树脂溶液后加以干燥而得到的挠性基板(例如参照专利文献1、2)、在玻璃表面贴附有树脂膜的挠性基板(例如参照专利文献3)。但是，即使使用这些技术，但在要求高温高湿下有高可靠性的显示装置的制造工序中，也无法获得满足充分的耐冲击性的挠性基板。
另外，在玻璃表面涂布树脂溶液后加以干燥而得到的挠性基板存在如下的问题：树脂溶液在涂布工序以及干燥工序时发泡，外观变差。另一方面，在玻璃表面贴附有树脂膜的挠性基板存在如下的问题：由于没有对玻璃充分附加提高玻璃的耐冲击性所需要的应力，因此无法获得充分的耐冲击性。此外，为了贴附树脂膜，当使用树脂溶液或者溶剂作为粘接剂时，膜上容易产生皱褶。膜的皱褶除了成为挠性基板的外观上的问题以外，当实施不使该皱褶产生的处置时，会产生膜断裂的问题。
现有技术文献
专利文献
专利文献1：日本特开平11-329715号公报
专利文献2：日本特开2008-107510号公报
专利文献3：日本特开2007-010834号公报
发明内容
发明欲解决的技术问题
本发明是为了解决上述以往的技术问题而完成的发明，其目的在于提供一种弯曲性、挠性、耐冲击性以及外观优异的透明基板的制造方法。
用于解决技术问题的方法
本发明的透明基板的制造方法包含：工序A，在具有溶剂透过性的支撑基材上涂布热塑性树脂(A)组合物溶液，形成涂布层；工序B，将无机玻璃的至少一个面与该涂布层经由粘接剂组合物贴合，形成层叠体；工序C，对该层叠体实施第1热处理，使该涂布层中的残留溶剂量减少至规定量；和，工序D，将该支撑基材从该层叠体上剥离后，进行第2热处理，使该涂布层干燥，形成热塑性树脂层。
在优选的实施方式中，上述涂布层形成时的该涂布层中的溶剂量为7重量％以上。
在优选的实施方式中，通过上述第1热处理，使上述涂布层中的残留溶剂量减少至15重量％以下。
在优选的实施方式中，将上述支撑基材剥离时的上述涂布层的收缩应力为10MPa以下。
在优选的实施方式中，在上述第2热处理后对无机玻璃附加的应力为10MPa～30MPa。
在优选的实施方式中，上述第1热处理的温度相对于上述热塑性树脂(A)组合物溶液中含量最多的溶剂的沸点(bpA)为(bpA-60)℃～(bpA+40)℃。
在优选的实施方式中，上述第2热处理的温度相对于上述热塑性树脂(A)组合物溶液中含量最多的溶剂的沸点(bpA)为(bpA-20)℃～250℃。
在优选的实施方式中，上述粘接剂组合物含有溶剂，该粘接剂层中的溶剂的沸点为上述热塑性树脂(A)组合物溶液中所含的溶剂的沸点以上。
在优选的实施方式中，上述粘接剂组合物含有溶剂，该粘接剂层中的溶剂对热塑性树脂(A)组合物溶液中所含的热塑性树脂(A)显示出溶解性。
在优选的实施方式中，上述粘接剂组合物含有与热塑性树脂(A)组合物溶液中所含的热塑性树脂(A)显示出相容性的成分。
在优选的实施方式中，上述粘接剂组合物含有溶剂、与上述热塑性树脂(A)组合物溶液显示出相容性的热塑性树脂(B)、热固性单体以及固化反应催化剂。
在优选的实施方式中，上述热塑性树脂(B)在末端具有反应基。
在优选的实施方式中，上述支撑基材在90℃下的储能模量为1.0×107Pa以上。
在优选的实施方式中，上述无机玻璃的厚度为100μm以下。
发明效果
通过本发明，对通过将在具有溶剂透过性的支撑基材上形成的包含溶剂的涂布层(即半干燥状态的涂布层)与无机玻璃经由粘接剂组合物贴合得到的层叠体实施热处理，使涂布层中的残留溶剂量减少至规定量，其后将支撑基材从该层叠体上剥离，再次进行热处理使涂布层干燥，由此可获得具有充分地附加了应力的无机玻璃以及发泡得到抑制的热塑性树脂层、且弯曲性、挠性、耐冲击性以及外观优异的透明基板。
附图说明
图1是示意地表示本发明的优选的实施方式的透明基板的制造方法的概略图。
图2是示意地表示本发明的另一优选的实施方式的透明基板的制造方法的概略图。
图3是通过本发明的制造方法得到的透明基板的概略截面图。
具体实施方式
图1是示意地表示本发明的优选的实施方式的透明基板的制造方法的概略图。本发明的制造方法包含：工序A，在支撑基材10上涂布热塑性树脂(A)组合物溶液，形成涂布层20；工序B，将无机玻璃30的至少一个面(在图示例中为无机玻璃30的两个面)与涂布层20经由粘接剂组合物40贴合，形成层叠体；工序C，对该层叠体实施第1热处理，使上述涂布层中的残留溶剂减少至规定量；和，工序D，将支撑基材10从该层叠体上剥离后，进行第2热处理，使涂布层20干燥，形成热塑性树脂层21。在本发明的制造方法中，涂布层20在工序A～工序C中为含有溶剂的半干燥状态，在其后的工序D中，为剥离了支撑基材10的状态，溶剂的干燥结束后形成热塑性树脂层21。通过本发明的制造方法，能够获得具有无机玻璃30、使粘接剂组合物40干燥而得到的粘接剂层41、和使包含热塑性树脂(A)的涂布层20干燥而得到的热塑性树脂层21的透明基板。
图2是示意地表示本发明的另一优选的实施方式的透明基板的制造方法的概略图。图2是表示将无机玻璃30的一个面与涂布层20经由粘接剂组合物40贴合时的实施方式。
A.工序A
工序A是在支撑基材上涂布热塑性树脂(A)组合物溶液、形成涂布层的工序。
上述支撑基材优选对上述热塑性树脂(A)组合物溶液的溶剂以及后述的粘接剂组合物中所含的溶剂具有耐溶剂性。作为构成这样的支撑基材的材料，例如可列举聚对苯二甲酸乙二醇酯(PET)、聚萘二甲酸乙二醇酯(PEN)等。
上述支撑基材具有溶剂透过性。优选上述支撑基材对上述热塑性树脂(A)组合物溶液的溶剂具有溶剂透过性。进一步优选对上述热塑性树脂(A)组合物溶液的溶剂以及后述的粘接剂组合物中所含的溶剂具有溶剂透过性。若使用这样的支撑基材，则在后续工序(工序C)中进行第1热处理而使溶剂挥发时，溶剂透过支撑基材，因此可在第1热处理时防止涂布层发泡。作为构成这样的支撑基材的材料，例如可列举未实施硅处理等表面处理的聚对苯二甲酸乙二醇酯(PET)。其中，在本说明书中，“溶剂透过性”的有无例如可通过以下方式来判断。即，对装入有10g溶剂的玻璃瓶(直径3.5cm×高度7.5cm)内进行氮置换，将该玻璃瓶的口用支撑基材封住后，将该装入有溶剂的玻璃瓶在((溶剂的沸点)-(35～45))℃的加热板上进行2小时的加热时，当在该玻璃瓶和/或支撑基材的内侧不产生冷凝时，判断为该支撑体对该溶剂具有“溶剂透过性”。
上述支撑基材在90℃下的储能模量优选为1.0×107Pa以上，进一步优选为1.0×107Pa～1.0×1010Pa。若为该范围，则可良好地保持上述涂布层，可获得无外观上之不均的透明基板。
上述支撑基材的厚度优选为25μm～120μm，进一步优选为50μm～100μm。若为该范围，则可良好地保持上述涂布层，可获得无外观上之不均的透明基板。
上述热塑性树脂(A)组合物溶液含有热塑性树脂(A)以及溶剂。
作为上述热塑性树脂(A)，可列举聚醚砜系树脂、聚碳酸酯系树脂、环氧系树脂、丙烯酸系树脂、聚对苯二甲酸乙二醇酯、聚萘二甲酸乙二醇酯等聚酯系树脂；聚烯烃系树脂、降冰片烯系树脂等环烯烃系树脂；聚酰亚胺系树脂、聚酰胺系树脂、聚酰亚胺酰胺系树脂、聚芳酯系树脂、聚砜系树脂、聚醚酰亚胺系树脂等。
上述热塑性树脂(A)的玻璃转移温度优选为150℃～350℃，进一步优选为170℃～330℃，特别优选为190℃～300℃。
上述热塑性树脂(A)组合物溶液中所含的溶剂只要可溶解热塑性树脂(A)，则可采用任意适宜的溶剂。作为该溶剂，例如可列举甲苯、二甲苯等芳香族系溶剂；环戊酮、甲基异丁酮等酮系溶剂；四氢呋喃、丙二醇甲醚等醚系溶剂；二氯甲烷、三氯乙烷等卤素系溶剂。这些溶剂可单独使用也可将2种以上组合使用。
上述热塑性树脂(A)组合物溶液的热塑性树脂(A)的浓度只要涂布作业可良好地进行，则可设定为任意适宜的浓度。
作为在上述支撑基材上涂布热塑性树脂(A)组合物溶液的方法，例如可列举气刀涂布法、刮涂法、刀涂法、反涂法、传送辊涂布法、凹版辊式涂布法、吻合式涂布法、铸涂法、喷洒式涂布法、孔缝式涂布法、压光涂布法、电镀涂布法、浸涂法、模涂法等涂布法；柔版印刷法等凸版印刷法、直接凹板印刷法、间接凹版印刷法等凹版印刷法、胶版印刷法等平版印刷法、丝网印刷法等孔版印刷法等印刷法等。
工序A中的涂布层的厚度优选为15μm～40μm，进一步优选为20μm～30μm。
上述涂布层形成时的涂布层中的溶剂量(即工序A中的涂布层中的溶剂量)优选为7重量％以上，进一步优选为7重量％～50重量％，特别优选为8重量％～40重量％，最优选为11重量％～30重量％。在工序A中的涂布层中的溶剂量少于7重量％时，在后续工序(工序C)的第1热处理时，有由于接触粘接剂组合物中的溶剂而在涂布层上产生溶剂裂痕的顾虑。另外，在多于50重量％时，涂布层的流动性变强，有在后续工序(工序B)中将涂布层与无机玻璃贴合时的作业性变差的顾虑。
工序A中的涂布层中的溶剂量例如可通过控制热塑性树脂(A)组合物溶液中的溶剂的种类以及溶剂量来进行调整。另外，也可视需要在涂布热塑性树脂(A)组合物溶液后，使规定量的溶剂挥发来调整涂布层中的溶剂量。在一个实施方式中，通过将涂布有溶剂量为70重量％以上的热塑性树脂(A)组合物溶液的支撑基材在20℃～100℃的环境温度下放置30秒～10分钟，可形成溶剂量为7重量％以上的涂布层。
B.工序B
工序B是将无机玻璃的至少一个面与上述涂布层经由粘接剂组合物贴合来形成层叠体的工序。
上述无机玻璃若为片状，则可采用任意适宜的无机玻璃。上述无机玻璃可为长条状，也可为单片状。上述无机玻璃根据组成的不同进行分类，例如可列举钠钙玻璃、硼酸玻璃、铝硅酸盐玻璃、石英玻璃等。另外，根据碱成分的不同进行分类，可列举无碱玻璃、低碱玻璃。上述无机玻璃的碱金属成分(例如Na2O、K2O、Li2O)的含量优选为15重量％以下，进一步优选为10重量％以下。
上述无机玻璃的厚度优选为100μm以下，进一步优选为20μm～90μm，特别优选为30μm～80μm。在本发明中，通过在无机玻璃的单侧或者两侧形成热塑性树脂层，可使无机玻璃的厚度变薄。
上述无机玻璃在波长550nm下的透射率优选为85％以上。上述无机玻璃在波长550nm下的折射率ng优选为1.4～1.65。
上述无机玻璃的密度优选为2.3g/cm3～3.0g/cm3，进一步优选为2.3g/cm3～2.7g/cm3。若为上述范围的无机玻璃，则可获得轻量的透明基板。
上述无机玻璃的成形方法可采用任意适宜的方法。代表性地上述无机玻璃可通过如下方式制作：将含有二氧化硅或氧化铝等主原料、芒硝或氧化锑等消泡剂以及碳等还原剂的混合物在1400℃～1600℃的温度下熔融，成形为薄片状之后，加以冷却来制作。作为上述无机玻璃的薄片成形方法，例如可列举流孔下引法(slot down draw)、熔融法、浮法等。通过这些方法而成形为片状的无机玻璃为了薄片化或提高平滑性，也可视需要利用氢氟酸等溶剂进行化学研磨。
上述无机玻璃可直接使用市售的无机玻璃，或者将市售的无机玻璃研磨到所期望的厚度后使用。作为市售的无机玻璃，例如可列举Corning公司制造的“7059”、“1737”或者“EAGLE2000”、旭硝子公司制造的“AN100”、NH TECHNO GLASS公司制造的“NA-35”、日本电气硝子公司制造的“OA-10”、SCHOTT公司制造的“D263”或者“AF45”等。
上述无机玻璃优选预先对一个面或者两个面实施偶联处理。若对无机玻璃进行了偶联处理，则可获得无机玻璃与粘接剂层的密合性优异的透明基板。作为偶联处理中使用的偶联剂，可列举环氧末端偶联剂、含有氨基的偶联剂、含有甲基丙烯酸基的偶联剂、含有巯基的偶联剂等。
上述粘接剂组合物优选为含有与上述热塑性树脂(A)显示出相容性的成分。若使用这样的粘接剂组合物，则可获得粘接剂层与热塑性树脂层的密合性优异的透明基板。
上述粘接剂组合物优选含有与热塑性树脂(A)显示出相容性的热塑性树脂(B)。作为热塑性树脂(B)的具体例子，可列举聚醚砜系树脂、聚碳酸酯系树脂、环氧系树脂、丙烯酸系树脂、聚对苯二甲酸乙二醇酯、聚萘二甲酸乙二醇酯等聚酯系树脂；聚烯烃系树脂、降冰片烯系树脂等环烯烃系树脂；聚酰亚胺系树脂、聚酰胺系树脂、聚酰亚胺酰胺系树脂、聚芳酯系树脂、聚砜系树脂、聚醚酰亚胺系树脂等树脂。其中，作为上述热塑性树脂(B)，优选使用与上述热塑性树脂(A)不同的树脂。
上述热塑性树脂(B)优选在末端具有反应性高的官能团。例如可列举羟基、酚性羟基、丙烯酸基、甲基丙烯酸基、烯丙基、乙烯基、巯基、烷氧基甲硅烷基、异氰酸酯基、氨基、羧酸基等。其中优选为酚性羟基。
上述热塑性树脂(B)的含量可根据所期望的粘接剂组合物的粘度来设定为任意适宜的值。上述粘接剂组合物在25℃下的粘度优选为0.1mPa·s～1000000mPa·s，进一步优选为0.2mPa·s～500000mPa·s，特别优选为0.3mPa·s～300000mPa·s。若为这样的范围，则将无机玻璃与上述涂布层经由粘接剂组合物贴合时的作业性优异。
上述粘接剂组合物优选含有热固性单体以及固化反应催化剂。若含有热固性单体以及固化反应催化剂，则可获得无机玻璃与粘接剂层、以及粘接剂层与热塑性树脂层的密合性更优异的透明基板。
作为上述热固性单体，例如可列举环氧系单体、环氧丙烷系单体、丙烯酸系单体、聚硅氧烷系单体等。这些热固性单体可单独使用也可将2种以上组合使用。其中优选为环氧系单体或者环氧丙烷系单体。若为这样的热固性单体，则例如当上述热塑性树脂(B)具有酚性羟基时，可形成与该热塑性树脂(B)强有力的相互作用，且可获得无机玻璃与粘接剂层、以及粘接剂层与热塑性树脂层的密合性更优异的透明基板。
上述热固性单体的含有比例相对于上述热塑性树脂(B)优选为10重量％～50重量％，进一步优选为12重量％～40重量％，特别优选为15重量％～35重量％。若为这样的范围，则可获得无机玻璃与粘接剂层、以及粘接剂层与热塑性树脂层的密合性更优异、且着色较少的透明基板。
上述固化反应催化剂优选为咪唑系催化剂、锡系催化剂或者钛系催化剂。这些催化剂可单独使用也可将2种以上组合使用。
作为上述咪唑系催化剂的具体例子，可列举2-甲基咪唑、1,3-二甲基咪唑、2-乙基4-甲基咪唑、2-十一烷基咪唑、2-十七烷基咪唑、2-苯基咪唑、2-苯基-4-甲基咪唑、1-苄基-2-甲基咪唑、1-苄基-2-苯基咪唑、1-氰乙基-2-甲基咪唑、1-氰乙基-2-乙基4-甲基咪唑等。
作为上述锡系催化剂的具体例子，可列举二丁基二月桂酸锡、二丁基二乙酸锡、二辛基二月桂酸锡、双(乙酰氧基二丁基锡)氧化物等。
作为上述钛系催化剂的具体例子，可列举松本精密化学公司制造的“TA-25”、“TC-750”等。
上述固化反应催化剂的含有比例相对于热塑性树脂(B)优选为1重量％～10重量％，进一步优选为2重量％～8重量％，特别优选为3重量％～5重量％。若为这样的范围，则可获得无机玻璃与粘接剂层、以及粘接剂层与热塑性树脂层的密合性更优异、且着色较少的透明基板。
上述粘接剂组合物优选含有溶剂。粘接剂组合物中所含的溶剂优选对上述热塑性树脂(A)也显示出溶解性。若粘接剂组合物含有这样的溶剂，则粘接剂组合物变得容易浸透至上述涂布层中，可获得粘接剂层与热塑性树脂层的密合性优异的透明基板。作为粘接剂组合物中所含的溶剂，优选使用与上述热塑性树脂(A)组合物溶液中所含的溶剂相同的溶剂。
上述粘接剂组合物中所含的溶剂的沸点优选与上述热塑性树脂(A)组合物溶液中所含的溶剂的沸点为同等以上。若粘接剂组合物中所含的溶剂的沸点与上述热塑性树脂(A)组合物溶液中所含的溶剂的沸点为同等以上，则在后续工序(工序C以及D)的第1热处理以及第2热处理时，粘接剂组合物中所含的溶剂的挥发难以被热塑性树脂(A)组合物溶液中所含的溶剂阻碍，因此可防止粘接剂组合物的发泡，获得外观优异的透明基板。
作为将上述无机玻璃与上述涂布层经由粘接剂组合物贴合的方法，可采用任意适宜的方法。作为该贴合的方法，例如可列举下述方法：在将粘接剂组合物供给到以一定之间隙设置的2个辊之间的同时，使形成有涂布层的支撑基材与无机玻璃从其间通过。所供给的粘接剂组合物可为溶液状态也可为薄片状态。
C.工序C
工序C是对工序B中得到的层叠体实施第1热处理的工序。通过第1热处理，可使上述涂布层中的残留溶剂减少至规定量。另外，同时粘接剂组合物中的溶剂也减少。此外，在粘接剂组合物含有热固性单体的情况下，进行该热固性单体的固化反应。
作为上述第1热处理的方法，可采用任意适宜的方法。第1热处理例如可列举使用如下装置的热处理：空气循环式恒温烘箱、利用了微波或者远红外线等的加热器、被加热用于温度调节的辊、热管辊或者金属带等。
上述第1热处理的温度相对于上述热塑性树脂(A)组合物溶液中含量最多的溶剂的沸点(bpA)优选为(bpA-60)℃～(bpA+40)℃，进一步优选为(bpA-60)℃～(bpA+20)℃，特别优选为(bpA-50)℃～(bpA+20)℃，最优选为(bpA-45)℃～(bpA)℃。若为这样的温度范围，则在第1热处理时，可防止上述涂布层以及粘接剂组合物发泡。其中，在第1热处理中，可阶段性地提高温度。
上述第1热处理的时间优选为1分钟～30分钟，进一步优选为5分钟～20分钟。
优选通过上述第1热处理，使上述涂布层中的残留溶剂量减少至15重量％以下。进一步优选减少至3重量％～15重量％，特别优选减少至4重量％～14重量％，最优选减少至5重量％～13重量％。当第1热处理后的涂布层中的残留溶剂量多于15重量％时，上述层叠体存在如下顾虑：在后续工序(工序D)中，搬送中的层叠体变得无法耐受施加于该层叠体的张力而断裂。
D.工序D
工序D是将上述支撑基材从上述层叠体上剥离后、进行第2热处理的工序。通过第2热处理，可使涂布层干燥，形成热塑性树脂层。另外，同时可使粘接剂组合物的干燥和/或固化结束而形成粘接剂层。
对于上述层叠体中的上述涂布层，通过上述工序C中的第1热处理而使涂布层中的溶剂挥发，由此施加收缩应力。将上述支撑基材剥离时的上述涂布层的收缩应力优选为10MPa以下，进一步优选为8MPa以下。若为这样的范围，可防止基材产生皱褶。另外，当基材产生皱褶时，有皱褶被转印至涂布层而获得外观上欠佳的透明基板的顾虑。
上述第2热处理的方法可采用与上述第1热处理相同的方法。
上述第2热处理的温度相对于上述热塑性树脂(A)组合物溶液中含量最多的溶剂的沸点(bpA)优选为(bpA-20)℃～250℃，进一步优选为(bpA-10)℃～200℃，特别优选为(bpA)℃～180℃。上述第2热处理的时间可设定为与上述第1热处理的时间相同的时间。
通过进行上述第2热处理，可将使涂布层干燥而得到的热塑性树脂层的收缩应力附加于无机玻璃。具有如此地附加有应力的无机玻璃的透明基板的弯曲性、挠性以及耐冲击性优异。
在上述第2热处理后附加于无机玻璃上的应力(即附加于通过本发明的制造方法得到的透明基板的无机玻璃的应力)优选为10MPa～30MPa，进一步优选为12MPa～30MPa，特别优选为15MPa～30MPa。若为这样的范围，则可获得无机玻璃与粘接剂层充分密合，且弯曲性、挠性以及耐冲击性优异的透明基板。更详细而言，当无机玻璃受到拉伸方向的外力时，由于拉伸应力集中于裂痕，无机玻璃会发生断裂，但通过本发明的制造方法得到的透明基板的无机玻璃由于附加有涂布层以及粘接剂层的收缩所产生的应力，因此裂痕所受到的拉伸应力减小。其结果，即使在更大的拉伸方向的外力下，也能够防止无机玻璃的裂痕发生进展和断裂，能够获得弯曲性、挠性以及耐冲击性优异的透明基板。
E.透明基板
图3是通过本发明的制造方法得到的透明基板的概略截面图。该透明基板200具有无机玻璃30、配置在无机玻璃30的一侧或者两侧(优选如图示例那样为两侧)的热塑性树脂层21，且在无机玻璃30与热塑性树脂层21之间进一步具有粘接剂层41。
本发明的透明基板可视需要在上述热塑性树脂层的与无机玻璃相反的一侧具有任意适宜的其它层。作为上述其它层，例如可列举透明导电性层、硬涂层等。
上述透明基板的总厚优选为150μm以下，进一步优选为140μm以下，特别优选为80μm～130μm。
在上述透明基板上引入裂痕而使其弯曲时的断裂直径优选为40mm以下，进一步优选为30mm以下。
上述透明基板在波长550nm下的透光率优选为80％以上，进一步优选为85％以上。优选上述透明基板在180℃下实施2小时的加热处理后的透光率的减少率为5％以内。其原因在于：若为这样的减少率，则即使在FPD的制造工艺中实施必要的加热处理，也可确保实用上可容许的透光率。
上述透明基板的表面粗度Ra(实质上为上述热塑性树脂层或者上述其它层的表面粗度Ra)优选为50nm以下，进一步优选为30nm以下、特别优选为10nm以下。上述透明基板的起伏优选为0.5μm以下，进一步优选为0.1μm以下。
上述透明基板的线膨胀系数优选为15ppm/℃以下，进一步优选为10ppm/℃以下，特别优选为1ppm/℃～10ppm/℃。上述透明基板由于具有上述无机玻璃，因此显示出优异的尺寸稳定性(例如如上所示的范围的线膨胀系数)。更具体而言，除了上述无机玻璃自身为刚性以外，由于上述热塑性树脂层受到该无机玻璃拘束，因此也能够抑制热塑性树脂层的尺寸变动。其结果，上述透明基板整体显示出优异的尺寸稳定性。
上述热塑性树脂层在波长550nm下的透光率优选为80％以上。上述热塑性树脂层在波长550nm下的折射率(nr)优选为1.3～1.7。
上述热塑性树脂层的厚度优选为5μm～80μm，进一步优选为8μm～60μm，特别优选为10μm～50μm。若为这样的范围，则热塑性树脂层可充分地强化无机玻璃。
上述热塑性树脂层的弹性模量优选为1.5GPa～10GPa以上，进一步优选为1.8GPa～9GPa，特别优选为2GPa～8GPa。
上述热塑性树脂层的断裂韧性值优选为1.5MPa·m1/2～10MPa·m1/2，进一步优选为2MPa·m1/2～6MPa·m1/2，特别优选为2.5MPa·m1/2～8MPa·m1/2。若为这样的范围，则可形成具有充分的粘着强度的热塑性树脂层，通过该热塑性树脂层可防止无机玻璃的裂痕的进展或断裂，能够获得具有良好的弯曲性的透明基板。另外，当将这样的包含热塑性树脂(A)的热塑性树脂层形成在无机玻璃两个面时，即使假设无机玻璃在透明基板内部发生断裂，热塑性树脂层也难以断裂，因此通过热塑性树脂层能够防止无机玻璃的飞散，且能够保持透明基板的形状，从而能够防止显示元件以及太阳电池在制造工序中设施发生污染，提高成品率。
上述粘接剂层的厚度优选为0.001μm～20μm，进一步优选为0.001μm～15μm，特别优选为0.01μm～10μm。若为这样的范围，则对透明基板的透明性的影响小，且即使在高温高湿的状况下也可表现出充分的粘接力。
当将上述透明基板作为照明元件、显示元件或者太阳电池的基板使用时，上述透明导电性层可作为电极或者电磁波屏蔽材料等发挥功能。
作为可用于上述透明导电性层的材料，例如可列举铜、银等金属；氧化铟锡(ITO)、氧化铟锌(IZO)等金属氧化物；聚噻吩、聚苯胺等导电性高分子；包含碳纳米管的组合物等。
上述硬涂层具有赋予上述透明基板以耐化学品性、耐擦伤性以及表面平滑性的功能。
作为构成上述硬涂层的材料，可采用任意适宜的材料。作为构成上述硬涂层的材料，例如可列举环氧系树脂、丙烯酸系树脂、聚硅氧烷系树脂以及它们的混合物。其中优选为耐热性优异的环氧系树脂。上述硬涂层可通过利用热或者活性能量线将这些树脂固化而得到。
实施例
以下，通过实施例对本发明加以具体之说明，但本发明并不受这些实施例的任何限定。其中，厚度是使用安立公司制造的数字式测微计“KC-351C型”测定的。另外，在实施例以及比较例中，作为支撑基材使用的PET基材的溶剂透过性是如下来判断的。
(PET基材的溶剂透过性)
在螺旋管瓶(As One公司制造、型号“No.7L”、件号“5-098011”、直径3.5cm×高度7.5cm)中放入环戊酮10g。其后，对该螺旋管瓶内进行氮置换，将该螺旋管瓶用5cm见方的PET基材封住。此时，用粘接剂(CemedineCo.,Ltd.制造、件号“AX-083”)将螺旋管瓶与PET基材粘接。然后，将该螺旋管瓶放置在加热至90℃的加热板上，进行2小时的加热。在加热结束后，目视观察PET基材以及螺旋管瓶的内侧的状态。
目视观察的结果，当在PET基材和/或螺旋管瓶的内侧产生溶剂的冷凝时，判断为该PET基材无溶剂透过性。另一方面，当不产生冷凝时，判断为该PET基材具有溶剂透过性。
[制造例1]
在具有搅拌装置的反应容器中，使4,4'-(1,3-二甲基亚丁基)双酚7.65g(0.028mol)、4,4'-(1-苯基亚乙基)双酚12.35g(0.043mol)、苄基三乙基氯化铵0.444g、对叔丁基苯酚0.022g溶解于1M氢氧化钠溶液185g中。在该溶液中一面搅拌一面一次性添加在氯仿246g中溶解有对苯二甲酰氯14.4g(0.071mol)的溶液，在室温下搅拌120分钟。其后，对聚合溶液进行静置分离而分离含有聚合物的氯仿溶液，接着用乙酸水溶液加以清洗，并用离子交换水加以清洗后，投入至甲醇中使聚合物析出。对析出的聚合物进行过滤，在减压下进行干燥，获得白色的聚合物27g。
[实施例1]
将经末端羟基改性的聚醚砜(SUMIKAEXCEL 5003P：住友化学公司制造)10g加热溶解于环戊酮90g中，获得10重量％的溶液。向得到的溶液中添加3-乙基-3{[(3-乙基环氧丙烷-3-基)甲氧基]甲基}环氧丙烷(ARONEOXETANE OXT-221：东亚合成公司制造)0.6g、1,2-二甲基咪唑0.4g、以及环氧末端偶联剂(KBM403：信越化学工业公司制造)2.5g，获得粘接剂组合物。
另外，将无机玻璃(厚度50μm、长度10cm×宽度4cm)的一个表面用甲乙酮加以清洗后，进行电晕处理，涂布环氧偶联剂(KBM403：信越化学工业公司制造)2％水溶液，在100℃下干燥10分钟。对无机玻璃的另一面也进行同样的处理。
其后，将在环戊酮90g中溶解有制造例1中得到的聚合物10g的10重量％的热塑性树脂(A)溶液涂布到具有溶剂透过性的PET(Lumirror：日本东丽股份有限公司制造、厚度为75μm)基材上，在90℃下使溶剂挥发8分钟，形成涂布层。涂布层中的溶剂量为23重量％(热塑性树脂(A)的浓度：77重量％)。
一面向上述无机玻璃与形成在上述PET基材上的涂布层之间供给上述粘接剂组合物，一面将无机玻璃与涂布层贴合。对无机玻璃的两个面进行这样的操作，获得层叠体(PET基材/涂布层/粘接剂组合物/无机玻璃/粘接剂组合物/涂布层/PET基材)。
对得到的层叠体在90℃下进行4分钟的热处理、在130℃下进行4分钟的热处理、在150℃下进行4分钟的热处理。该热处理后的涂布层中的残留溶剂量为6重量％。
其后，将两个面的PET基材剥离，进而在150℃下进行12分钟的热处理，获得总厚度为115μm的透明基板(热塑性树脂层(30μm)/粘接剂层(2.5μm)/无机玻璃(50μm)/粘接剂层(2.5μm)/热塑性树脂层(30μm))。其中，无机玻璃露出于上述透明基板的宽度方向端部(长度10cm×宽度1cm)。
[实施例2]
在粘接剂组合物中进一步添加二丁基二月桂酸锡0.05g，除此以外与实施例1同样地进行，获得透明基板。
[比较例1]
将形成涂布层时的涂布层中的溶剂量定为6重量％(热塑性树脂层(A)的浓度为94重量％)，除此以外与实施例1同样地进行，获得透明基板。
[比较例2]
使用进行了硅处理的不具溶剂透过性的PET(MRF：三菱树脂股份有限公司制造、厚度为38μm)基材代替具有溶剂透过性的PET(Lumirror：日本东丽股份有限公司制造、厚度为75μm)基材，除此以外与实施例1同样地进行，获得透明基板。
[比较例3]
在层叠体形成后(即在热处理前)立即将PET基材剥离，除此以外与实施例1同样地进行，获得透明基板。
[比较例4]
将在环戊酮600g中溶解有制造例1中得到的聚合物90g的流延溶液涂布到PET(Lumirror：日本东丽股份有限公司制造、厚度为75μm)基材上，进而进行干燥直至残留溶剂量为5％以下，然后将基材剥离，获得聚芳酯膜。
另外，将无机玻璃(厚度为50μm、长度10cm×宽度4cm)的一个表面用甲乙酮加以清洗后，进行电晕处理，用环氧偶联剂(KBM403：信越化学工业公司制造)进行处理。对无机玻璃的另一面也进行同样的处理。
使用含有3,4-环氧环己烯基甲基-3',4'-环氧环己烯羧酸酯(Celloxide2021P：DAICEL CHEMICAL INDUSTRIES,LTD.制造)8g、3-乙基-3{[(3-乙基环氧丙烷-3-基)甲氧基]甲基}环氧丙烷(ARONE OXETANE OXT-221：东亚合成公司制造)2g、光聚合起始剂(SP-170：ADEKA公司制造)0.4g的粘接剂组合物在上述无机玻璃的两个面贴合上述聚芳酯膜后，进行UV照射而使粘接剂组合物固化，获得透明基板(聚芳酯膜层/粘接剂层/无机玻璃/粘接剂层/聚芳酯膜层)。其中，无机玻璃露出于上述透明基板的宽度方向端部(长度10cm×宽度1cm)。
[比较例5]
将经末端羟基改性的聚醚砜(SUMIKAEXCEL 5003P：住友化学公司制造)36.2g溶解于环戊酮172g以及N,N-二甲基甲酰胺10.8g的混合溶剂中，获得聚醚砜为16.5重量％的溶液。进而向该溶液中添加流平剂(BYK307，BYK Chemie公司制造)0.027g、3,4-环氧环己烯基甲基-3',4'-环氧环己烯羧酸酯(Celloxide 2021P：DAICEL CHEMICAL INDUSTRIES,LTD.制造)1.81g、3-乙基-3{[(3-乙基环氧丙烷-3-基)甲氧基]甲基}环氧丙烷(ARONEOXETANE OXT-221：东亚合成公司制造)1.45g、2-甲基咪唑1.09g、环氧末端偶联剂(KBM403：信越化学工业公司制造)9.05g，获得第1流延溶液。
另外，将无机玻璃(厚度为50μm、长度10cm×宽度4cm)的一个表面用甲乙酮加以清洗后，进行电晕处理，涂布添加有偶联剂等的流延溶液，在100℃下干燥10分钟，进而在170℃下干燥20分钟，形成厚度为1μm的第1热塑性树脂层。对无机玻璃的另一面也进行同样的处理。
其后，将在环戊酮600g中溶解有制造例1中得到的聚合物90g的第2流延溶液涂布到第1热塑性树脂层上，在90℃下干燥15分钟。另外在背面也将第2流延溶液涂布到第1热塑性树脂层上，在85℃下干燥10分钟，其后使两个面在130℃下干燥10分钟，进而在170℃下干燥20分钟，获得单侧的厚度为36.5μm的第2热塑性树脂，获得总厚度为125μm的透明基板(第2热塑性树脂层/第1热塑性树脂层/无机玻璃/第1热塑性树脂层/第2热塑性树脂层)。其中，无机玻璃露出于上述透明基板的宽度方向端部(长度10cm×宽度1cm)。
<评价>
通过下述方法而评价上述得到的透明基板。将结果示于表1。
(1)密合性试验
通过JIS K 5400的网格剥离试验(cross-cut peeling test)进行评价。即，在得到的透明基板以及层叠体的一个最外层的表面上的10mm见方中，以1mm之间隔通过切割机引入缝隙，制作100个网格，在其上贴附粘着带后进行剥离，根据从无机玻璃上剥离的树脂层的网格数来评价密合性。
(2)外观
目视确认得到的透明基板的外观。将透明基板上确认不到发泡、裂痕、皱褶的情况记为合格(表1中以○表示)。
(3)断裂直径
(a)准备实施例以及比较例中得到的透明基板作为评价用试样。
(b)在薄片玻璃露出部分的长边中央切入5mm以下的裂痕。
(c)使评价用试样的长边弯曲，观察裂痕的进展，将玻璃断裂时的以弯曲的边(长边)为圆周的圆的直径作为断裂直径。
(4)收缩应力
在宽度30mm×长度125mm的条状无机玻璃(厚度为100μm)的一个面上，通过与实施例以及比较例同样的方法而形成树脂层，测定卷曲的样本的曲率半径R。
在导入有校正项的Stonry的下式(C.A.Klien,J.Appl.Phys.,885487(2000))中代入曲率半径R；薄片玻璃的杨氏模量(70GPa)、帕松比(0.2)以及厚度(100μm)；树脂的杨氏模量、帕松比以及厚度，求出树脂层的收缩应力(即附加于无机玻璃的应力)。
[数学式1]
σ＝((1+χδ3)/(1+δ))*(E's*ts 2/(6*R*tf))
～(1/(1+δ))*(E's*ts 2/(6*R*tf))
σ：收缩应力(MPa)  σ：tf/ts
χ：E'f/E's         tf：玻璃的厚度(μm)
E'f：Ef/(1-γf)     ts：树脂层的厚度(μm)
E's：Es/(1-γs)     R：曲率半径(μm)
Ef：树脂的杨氏模量(MPa)
γf：树脂的帕松比
Es：玻璃的杨氏模量(MPa)
γs：玻璃的帕松比
[表1]
根据表1可知：实施例1以及2的透明基板由于对具有支撑基材、粘接剂组合物、包含有规定量的溶剂的涂布层的层叠体进行第1热处理，其后将支撑基材剥离并进行第2热处理，因此密合性优异、树脂层的收缩应力大、断裂直径小。这些表示通过本发明的制造方法得到的透明基板的弯曲性、挠性以及耐冲击性优异。另一方面，比较例4的透明基板的树脂层(聚芳酯膜层)的收缩应力小。这样的透明基板没有对无机玻璃附加充分的应力，弯曲性、耐冲击性差。
另外，通过实施例1以及2的制造方法获得了外观优异的透明基板。另一方面，在涂布层中的溶剂量少的状态下进行了第1热处理的透明基板(比较例1)产生裂痕。另外，当在形成层叠体后(即热处理前)立即将PET基材剥离时，在工序中断裂而无法制作透明基板(比较例3)。此外，当使用不具有溶剂透过性的PET基材作为支撑基材时(比较例2)、以及通过不使用支撑基材的以往方法的直接涂布来形成热塑性树脂层时，确认到发泡(比较例5)。
产业上的可利用性
通过本发明的制造方法得到的透明基板可用于显示元件、太阳电池或者照明元件中。作为显示元件，例如可列举液晶显示器、等离子体显示器、有机EL显示器、电子纸等。作为照明元件，例如可列举有机EL元件等。
符号说明
10        支撑基材
20        涂布层
30        无机玻璃
40        粘接剂组合物
21        热塑性树脂层
41        粘接剂层
100、100' 烘箱
200       透明基板

Claims (2)

1.一种层叠体，其具备无机玻璃以及通过涂布热塑性树脂(A)组合物溶液而形成的涂布层，
其中，该涂布层的残留溶剂量为3重量％～15重量％。
2.如权利要求1所述的层叠体，其是通过如下的方法形成的：
在具有溶剂透过性的支撑基材上涂布热塑性树脂(A)组合物溶液，形成涂布层，
然后，在将无机玻璃的至少一个面与该涂布层经由粘接剂组合物贴合后，对该层叠体实施第1热处理，使该涂布层中的残留溶剂量减少至规定量。
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EP2565170A1 (en) 2013-03-06
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US20130032277A1 (en) 2013-02-07
WO2011136327A1 (ja) 2011-11-03
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KR20130024902A (ko) 2013-03-08

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