CN101588922B - 透明层叠体及其制造方法 - Google Patents

透明层叠体及其制造方法 Download PDF

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Publication number
CN101588922B
CN101588922B CN2007800487133A CN200780048713A CN101588922B CN 101588922 B CN101588922 B CN 101588922B CN 2007800487133 A CN2007800487133 A CN 2007800487133A CN 200780048713 A CN200780048713 A CN 200780048713A CN 101588922 B CN101588922 B CN 101588922B
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China
Prior art keywords
resin composition
hardening resin
transparency carrier
pair
manufacture method
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CN2007800487133A
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CN101588922A (zh
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伊藤广茂
新山聪
菊地哲
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AGC Inc
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Asahi Glass Co Ltd
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    • 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
    • B32B17/10—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 of synthetic resin
    • B32B17/10005—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 of synthetic resin laminated safety glass or glazing
    • B32B17/1055—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 of synthetic resin laminated safety glass or glazing characterized by the resin layer, i.e. interlayer
    • B32B17/10706—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 of synthetic resin laminated safety glass or glazing characterized by the resin layer, i.e. interlayer being photo-polymerized
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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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    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
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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
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
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    • B29C66/001—Joining in special atmospheres
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • 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

本发明的目的在于消除采用透明树脂膜的透明层叠体的制造技术中的问题以及注入低粘性的树脂组合物所制造的透明层叠体的制造技术中的问题。在一对透明基板的一块透明基板上的周边部形成用于封入固化性树脂组合物的密封部，向透明基板上的以密封部围成的区域供给固化性树脂组合物，在减压气氛下在所供给的所述固化性树脂组合物上重叠另一块透明基板，在一对透明基板间夹持固化性树脂组合物并密封，再在比夹持时的气氛压力高的压力下使固化性树脂组合物固化，从而制成透明层叠体。

Description

透明层叠体及其制造方法
技术领域
本发明涉及如被用作建筑物或车辆等的窗用玻璃的夹层玻璃等在2块玻璃基板之间形成有树脂制的中间层的透明层叠体及其制造方法。
背景技术
已知介以聚乙烯醇缩丁醛(PVB)等的热塑性透明树脂膜或热交联性透明树脂膜，将一对透明基板通过高压釜进行加热、加压的同时粘合而构成的透明层叠体，透明基板为玻璃基板时以夹层玻璃的名称为人所知。这样的夹层玻璃由于破损的玻璃碎片附着于膜而不会飞散，所以被用作汽车的挡风玻璃，且因不易穿透、强度良好而被用作建筑物的窗玻璃(安全玻璃、防盗玻璃)。
然而，采用所述的透明树脂膜的透明基板的制造方法需要至少70℃以上或120℃以上的高温环境或者10大气压以上的高压，因此存在生产中的环境负荷大的问题。此外，因为同样的理由，也存在透明基板无法使用透明树脂基板等热变形耐受性差的透明基板。另外，根据透明基板的尺寸切割透明树脂膜时，例如修剪下的膜作为不需要的膜被废弃，因此还存在透明树脂膜的利用效率差的问题。
于是，作为解决这样的问题的夹层玻璃的制造方法，已知专利文献1等中所揭示的制法。该制法为如下的方法：首先，制作夹着粘接性的间隔物粘合一对玻璃基板而得的平板状的容器；接着，使间隔物的一部分开口，从该开口部分注入固化性树脂组合物；然后，堵塞间隔物的所述开口部后，通过加热(包括室温的长时间保持)或紫外线使固化性树脂组合物固化，从而制成夹层玻璃(以下称为注入法)。因此，如果采用该制法，则不需要高温环境、高压力环境，所以可以使用热变形耐受性差的透明基板，且因为也不使用成膜而得的透明树脂膜，所以可以节约资源。
专利文献1:日本专利特开2005-41747号公报
发明的揭示
然而，在向由一对透明基板形成的平板容器中注入固化性树脂组合物的专利文献1等的技术中，存在注入所产生的气泡的除去需要时间的问题。此外，固化性树脂组合物必须采用粘性低至可注入的程度的固化性树脂组合物，因此大量含有分子量较小的固化性化合物，因而固化性树脂组合物的固化前后的收缩率增大，所以存在无法充分获得作为夹层玻璃的强度的问题。
本发明的目的在于提供基板的种类不受限定，形成中间层的固化性树脂组合物的种类的自由度大，可以有效地利用用于形成中间层的资源，且不需要以往的注入法中所需的气泡除去步骤，生产性良好，环境负荷小的透明层叠体的制造方法及通过该制造方法制成的透明层叠体。还有，本发明中，“固化性树脂组合物”是指未固化状态的固化性树脂组合物，而以下将“固化性树脂组合物”固化而生成的固化物称为“固化了的固化性树脂组合物”，或者简称“固化树脂”。
为了实现所述目的，本发明提供一种透明层叠体的制造方法，该方法是具有一对透明基板和存在于所述一对透明基板间的固化性树脂组合物的固化物的层的透明层叠体的制造方法，其特征在于，在一块透明基板上的周边部形成用于封入固化性树脂组合物的密封部，向透明基板上的以所述密封部围成的区域供给固化性树脂组合物，在减压气氛下在所供给的所述固化性树脂组合物上重叠另一块透明基板，在一对透明基板间夹持固化性树脂组合物并密封，再将夹持有固化性树脂组合物的一对透明基板置于比所述减压气氛的压力高50kPa以上的压力气氛下，在所述压力气氛下使固化性树脂组合物固化；
所述密封部可以保持由该密封部和所述一对透明基板密闭而成的密闭空间的减压度；
所述固化性树脂组合物的25℃的粘度在0.2Pa·s以上，且40℃的粘度在50Pa·s以下。
该方法中，较好是所述一对透明基板是具有大致相同的曲率的弯曲基板。
该方法中，较好是与固化性树脂组合物接触的透明基板表面中的至少一个表面预先以选自硅烷化合物和钛化合物的偶联剂进行了处理。
该方法中，较好是在一对透明基板间夹持固化性树脂组合物的减压气氛为10～100Pa的压力气氛。
该方法中，较好是使固化性树脂组合物固化的压力气氛为大气压。
该方法中，较好是通过加热或紫外线照射使固化性树脂组合物固化。
该方法中，较好是固化性树脂组合物为包含至少1种每1分子具有1～3个选自丙烯酰氧基和甲基丙烯酰氧基的固化性基团的化合物和光聚合引发剂的光固化性的固化性树脂组合物。
本发明还提供一种透明层叠体，其特征在于，如下制成：在减压气氛下将固化性树脂组合物介以设置于透明基板的周边部而使所述固化性树脂组合物封入的密封部夹持在一对透明基板之间，并在比夹持时的气氛压力高的压力下使固化性树脂组合物固化。
本发明的透明层叠体中，所述透明基板较好是玻璃或树脂。
透明层叠体的透明基板是玻璃板时，可以提供被用作建筑物或车辆等的窗用玻璃的夹层玻璃。如果树脂制透明基板使用聚碳酸酯，则可以提供耐冲击性高且轻量的透明面板。该透明面板也可以用作建筑物或车辆等的窗用玻璃。此外，可以是将玻璃基板和树脂板以该固化性树脂组合物粘合而得的透明层叠体。
本发明的透明层叠体可以使用具有大致相同的曲率的弯曲基板作为所述一对透明基板。
使用膜作为中间层的以往的透明层叠体中，如果透明基板是一定曲率以上的弯曲基板，则膜产生皱褶，因此透明层叠体的制造困难，但通过使固化性树脂组合物固化而制成的本发明的透明层叠体的形状不受限制。因此，透明基板为立体形状上有较大弯曲的基板时，形成弯曲的透明层叠体，是非常有效的。
为了实现所述目的，本发明提供如下制造透明层叠体的方法：在减压气氛下将固化性树脂组合物介以设置于透明基板的周边部而使所述固化性树脂组合物封入的密封部夹持在一对透明基板之间，并在比夹持时的气氛压力高的压力下使固化性树脂组合物固化。
另外，本发明还提供具有一对透明基板和存在于该一对透明基板间的固化性树脂组合物的固化物的层的透明层叠体的制造方法，其特征在于，在一块透明基板上的周边部形成用于封入固化性树脂组合物的密封部，向透明基板上的以所述密封部围成的区域供给固化性树脂组合物，在减压气氛下在所供给的所述固化性树脂组合物上重叠另一块透明基板，在一对透明基板间夹持固化性树脂组合物并密封，再将夹持有固化性树脂组合物的一对透明基板置于比所述减压气氛高的压力的气氛下，在所述压力气氛下使固化性树脂组合物固化。
如果采用这些制造方法，则由于在减压气氛下以一对透明基板夹持固化性树脂组合物，在比夹持时的气氛压力高的压力下使固化性树脂组合物固化，因此不会产生注入所产生的气泡的除去需要时间的问题，而且即使一对透明基板在减压下层叠时存在少量未以树脂组合物充盈的空间，也可以通过保持于更高的压力下而将该空间微小化，或者使其实质上消失。此外，还可以容易地提供基于通过以往的注入法难以实现的薄树脂层的透明层叠体。
因此，通过这些制造方法制成的透明层叠体成为没有气泡的透明层叠体。此外，由于被设于透明基板的周边部的密封部完全地密封，因此所得的透明层叠体在其后的严酷的使用条件下也不易发生自周边部的剥落等，耐久性高。
此外，通过以上述制造方法制造透明层叠体，作为固化性树脂组合物，可以使用粘度高的组合物或分子量高的固化性化合物，所以固化时形成强度高的固化树脂，可以获得作为整体机械强度高的透明层叠体。因此，本发明的透明层叠体与注入低粘度的固化性树脂组合物而制成的以往的透明层叠体相比，即使厚度小，也可以获得足够的透明层叠体的机械强度。
本发明的制造方法中，所述一对透明基板可以使用具有大致相同的曲率的弯曲基板。以膜作为中间层而制造的以往的透明层叠体的制造方法中，如果透明基板是一定曲率以上的弯曲基板，则膜产生皱褶，因此透明层叠体的制造困难，但如果采用该制造方法，则所制成的透明层叠体的形状不受限制。因此，透明基板可以使用立体形状上有较大弯曲的基板，容易地制造弯曲的透明层叠体。
本发明的制造方法中，较好是与固化性树脂组合物接触的透明基板表面中的至少一个表面预先以选自硅烷化合物和钛化合物的偶联剂进行了处理。
由硅烷化合物形成的偶联剂被称为硅烷偶联剂，代表性的化合物是具有与硅原子结合的有机基团和与硅原子结合的水解性基团的化合物。由钛化合物形成的偶联剂被称为钛偶联剂，代表性的化合物是具有与钛原子结合的有机基团和与钛原子结合的水解性基团的化合物。将这些偶联剂作为表面处理剂，预先涂布于一对透明基板的至少一块的固化性树脂组合物接触的表面，采用加热等使其结合于透明基板表面。
通过使用这样预先进行了表面处理的透明基板，可以使固化了的固化性树脂组合物对透明基板的粘接性提高。因此，所得的透明层叠体的机械强度提高，所以适合于夹层玻璃的制造。
本发明的制造方法中，较好是在一对透明基板间夹持固化性树脂组合物的减压气氛为10～100Pa的压力气氛。
如果该压力P1超过100Pa，则残存于透明层叠体中的固化树脂层的气泡容易变得显著；如果该压力P1不足10Pa，则减压度高，因此构筑该减压气氛时的时间上的损失增加。此外，如果减压度过高，则固化性树脂组合物中所含的热聚合引发剂或光聚合引发剂、阻聚剂、光稳定剂等添加物在真空容器内部分地发生挥发等，可能会引起固化不良，或者对固化后的固化树脂层的性能造成不良影响，因此是不理想的。
本发明的制造方法中，较好是使固化性树脂组合物固化的压力气氛为大气压。
通过这样采用大气压作为比层叠时高的固化时的压力，可以省去用于使固化性树脂组合物固化的压力容器等设备。此外，减压气氛为10～100Pa的压力气氛时，可以使与减压气氛的压力差足够高。
本发明的制造方法中，较好是通过加热或紫外线照射使固化性树脂组合物固化。可通过加热而固化的固化性树脂组合物通常是包含固化性化合物和热聚合引发剂的热固性树脂组合物，可通过紫外线而固化的固化性树脂组合物通常是包含固化性化合物和光聚合引发剂的光固化性树脂组合物。
如果采用这样的制造方法，则热固性树脂组合物时加热，光固化性树脂组合物时照射紫外线即可。或者，可以选择可通过在室温下长时间保持而固化的固化性树脂组合物。作为固化性树脂组合物，特别好是可通过紫外线而固化的光固化性的固化性树脂组合物。例如，热固性树脂组合物包含丙烯酸酯等丙烯酸类固化性化合物时，为了诱发热聚合引发剂的引发反应，需要加热至例如80℃。另一方面，通过紫外线使包含丙烯酸类固化性化合物的光固化性的固化性树脂组合物固化时，仅通过照射紫外线即可实现，所以可以节能地使固化性树脂组合物固化。此外，紫外线固化的情况下，温度也不会上升，因此环境负荷小，即使是对热变形的耐受性弱的透明基板也可以使用。室温固化的情况下，需要为了固化而静置例如1天～数天，但紫外线固化的情况下，数分钟～数十分钟就可以使其实质上固化，生产效率高。此外，也可以通过并用紫外线和加热或者紫外线固化后在室温下保持一定时间来完成固化反应。
此外，固化性树脂组合物较好是固化后形成透明性高的固化树脂的固化性树脂组合物。固化性树脂组合物的固化后的透明性以所得的透明层叠体的雾度值表示，从确保透明层叠体的透明性的角度来看，较好是达到6％以下。另外，为了保持透明层叠体整体的透明性，用于所述密封部的固化性树脂组合物也较好是固化后形成透明性高的固化树脂的固化性树脂组合物。
本发明的制造方法中，较好是固化性树脂组合物的25℃的粘度在0.2Pa·s以上，且40℃的粘度在50Pa·s以下。
使用这样的粘度的固化性树脂组合物来制造透明层叠体的情况下，可以使用粘度高的固化性树脂组合物或包含分子量高的固化性化合物的固化性树脂组合物。为了使固化性树脂组合物的25℃的粘度不足0.2Pa·s，需要在组合物中添加一定量以上的低分子量的固化性化合物，因此固化前后的收缩大，固化树脂中残留应变，机械强度低。此外，如果40℃的粘度超过50Pa·s，则固化性树脂组合物的流动性低，因此例如即使在夹持固化性树脂组合物后放置于大气中，因为其流动性不佳，所以固化性树脂组合物扩散至透明基板的间隙整体为止也需要时间。因此，到透明基板的间隙内不存在固化性树脂组合物的空间消失为止需要较长时间，容易导致制造节拍的下降。从以上的粘度和分子量的角度来看，制造本发明的透明层叠体时，较好是包含分子量在1000以上的固化性化合物的40℃的粘度在50Pa·s以下的固化性树脂组合物。
本发明的制造方法中，较好是固化性树脂组合物为包含至少1种每1分子具有1～3个选自丙烯酰氧基和甲基丙烯酰氧基的固化性基团的化合物和光聚合引发剂的光固化性的固化性树脂组合物。
如前所述，作为本发明中的固化性树脂组合物，较好是可接受紫外线等光的照射而固化的固化性树脂组合物。该光固化性的固化性树脂组合物较好是包含具有丙烯酰氧基的化合物(即丙烯酸酯)或具有甲基丙烯酰氧基的化合物(即甲基丙烯酸酯)作为固化性化合物的固化性树脂组合物。此外，每1分子的这些固化性官能团的数量较好是1～3个。通过使固化性树脂组合物为包含这些固化性化合物的至少1种和光聚合引发剂的光固化性的固化性树脂组合物，通过采用所述紫外线等光的固化所带来的特点得到充分地发挥。
如果采用本发明的制造方法，可提供基板的种类不受限定，形成中间层的固化性树脂组合物的种类的自由度大，可以有效地利用用于形成中间层的资源，且不需要以往的注入法中所需的气泡除去步骤，生产性良好，环境负荷小的透明层叠体的制造方法及通过该制造方法制成的透明层叠体。
如果采用本发明，在减压气氛下通过一对透明基板夹持固化性树脂组合物，在比夹持时的气氛压力高的压力下使固化性树脂组合物固化，因此不会产生气泡，且所夹持的固化性树脂组合物包在预先设于周边的密封材料内，所以所用的固化性树脂组合物的利用效率高。
此外，由于制作层叠体时不需要高温和高压，因此环境负荷小。
另外，不需要像以往那样向以平板构成的空间内注入树脂，因此可以使用采用可提高固化树脂的强度的分子量较高的固化性化合物的高粘度的固化性树脂组合物。因此，可以获得适合作为夹层玻璃的强度。
另外，由于被设于透明基板的周边部的密封部完全地密封，因此在其后的严酷的使用条件下也不易发生自周边部的剥落等，耐久性高。
此外，还可以容易地提供基于通过以往的注入法难以实现的薄树脂层的层叠体。
附图的简单说明
图1是在透明基板的4个边缘部粘贴双面胶粘带的说明图，(A)为平面图，(B)为剖视图。
图2是在透明基板上涂布固化性树脂组合物的说明图，(A)为平面图，(B)为剖视图。
图3是意图将一对透明基板在减压下介以双面胶粘带密合的说明图。
图4是表示紫外线照射装置的简要结构的说明图。
图5是表示本发明的优选的透明层叠体的制造步骤的流程图。
符号的说明
10…透明基板，12…双面胶粘带(密封材料)，13…区域，14…固化性树脂组合物，16…透明基板，18…下平台，20…给料器，22…进给丝杠，24…进给丝杠，26…减压舱，28…真空泵，30…上平台，32…吸盘，34…汽缸，36…固化性树脂组合物，40…紫外线照射装置，42…高压汞灯，44…反射镜，46…反射镜，48…固化性树脂组合物处于未固化的状态的透明层叠体。
实施发明的最佳方式
本发明的透明基板的材料较好是玻璃或树脂。作为玻璃，较好是通常被用作建筑物或车辆等的窗材的钠钙玻璃。作为树脂材料，较好是聚碳酸酯或聚甲基丙烯酸甲酯等透明性高的树脂材料。透明基板的形状没有特别限定，较好是平板形状或弯曲平板形状等作为窗材所采用的形状。透明基板的尺寸没有特别限定。但是，由于本发明可以制造难以通过以往的固化性树脂注入法制造的大型的透明层叠体，透明基板和所得的透明层叠体的尺寸较好是600mm×600mm以上的尺寸。
透明基板较好是与固化性树脂组合物接触的透明基板表面中的至少一个表面预先以选自硅烷化合物和钛化合物的偶联剂进行了处理。由硅烷化合物形成的偶联剂被称为硅烷偶联剂，代表性的化合物是具有与硅原子结合的有机基团和与硅原子结合的水解性基团的化合物。由钛化合物形成的偶联剂被称为钛偶联剂，代表性的化合物是具有与钛原子结合的有机基团和与钛原子结合的水解性基团的化合物。与硅原子或钛原子结合的有机基团是其结合末端的原子为碳原子，该碳原子与这些金属原子结合的有机基团。具体来说，例如有烷基、链烯基、官能团结合烷基等。作为官能团，例如有丙烯酰氧基、甲基丙烯酰氧基、环氧基、氨基等。水解性基团是与水反应而生成羟基的基团，例如有烷氧基、氯原子、酰基、氨基等。
作为偶联剂，较好是作为具有与硅原子结合的官能团结合烷基和烷氧基的硅烷化合物的硅烷偶联剂。这些偶联剂较好是具有在固化性树脂组合物固化时可与固化性树脂组合物中的固化性化合物化学结合的官能团。作为这些官能团，可以例举丙烯酰氧基和甲基丙烯酰氧基。作为具体的硅烷偶联剂，可以例举例如3-甲基丙烯酰氧基丙基三甲氧基硅烷。
将这些偶联剂作为表面处理剂，预先涂布于一对透明基板的至少一块的固化性树脂组合物接触的表面，采用加热等使其结合于透明基板表面。认为通过该表面处理，偶联剂的水解性基团水解，藉由生成的羟基结合于基板表面。作为表面处理方法，可以例举例如以下的方法：将偶联剂溶解于溶剂而制成偶联剂溶液，将该溶液涂布于透明基板表面或将透明基板浸渍于该溶液后取出，加热而蒸发除去溶剂，然后加热而使偶联剂结合于透明基板表面。也可以使用将偶联剂溶解于溶剂后使偶联剂部分水解而得的溶液来代替偶联剂溶液。
具体来说，例如通过将硅烷偶联剂:水:iPA(异丙醇)=0.3:0.5:99.2的溶液在室温下搅拌10小时而使硅烷偶联剂水解，获得部分硅烷醇化的溶液，再将该溶液浸渍透明基板1分钟后取出，然后通过150℃的烘箱进行30分钟的热处理，使其与玻璃表面反应。
通过使用实施了上述表面处理的透明基板，固化树脂对透明基板的粘接性提高，透明层叠体的机械强度提高。
此外，上述一对透明基板可以是具有大致相同的曲率的弯曲基板。使用膜作为中间层的以往的透明层叠体中，如果透明基板是弯曲基板，则膜产生皱褶，因此透明层叠体可能会难以制造。通过在透明基板间夹持固化性树脂组合物并使其固化而制成的透明层叠体的形状不受限制。因此，即使作为透明基板使用立体形状上弯曲的基板，也可以获得良好的立体形状上弯曲的透明层叠体。这是通过以往的使用膜的夹层玻璃的制法无法实现的形态。
本发明的透明层叠体通过本发明的制造方法制成。以下，对本发明的制造方法及通过该方法得到的透明层叠体进行说明。
首先，取出一对透明基板中的一块透明基板，沿该块透明基板的周边部设置密封部。该密封部可以通过粘贴双面胶粘带等密封构件来设置。接着，向一方的透明基板的被所述密封部围起的区域供给固化性树脂组合物。固化性树脂组合物的供给量预先设定为通过密封部和一对透明基板所密封的空间恰好被固化性树脂组合物填充的量。这时，可以预先考虑到固化性树脂组合物的固化收缩产生的体积减少来确定固化后的树脂层的体积。关于供给方法，将一方的透明基板平放，通过如给料器或模涂机等供给装置呈点状、线状或面状供给即可。接着，在减压气氛下、例如真空(包括近似真空)气氛下，将另一块透明基板介以密封部重合，从而将固化性树脂组合物夹持于一对透明基板间并密封。随后，根据需要在该减压气氛下夹持固化性树脂组合物规定时间。然后，将所述减压气氛变为比该气氛高的压力(例如大气压)的气氛后，一对透明基板被上升了的压力压向相互密合的方向的同时，残留于上述密封了的空间的空孔部的体积因该气氛的差压而缩减，所以固化性树脂组合物流向由一对透明基板和密封部所密闭的密闭空间中的减压空间，密闭空间整体被固化性树脂组合物均匀地填充。然后，使固化性树脂组合物固化，从而制成本发明的透明层叠体。
为了使一对透明基板的粘接性提高，较好是预先在密封构件的与透明基板接触的一面或其两面涂布固化性树脂组合物。通过这样在密封构件的面上涂布固化性树脂组合物，所述的密闭空间的密闭度提高，所以从减压气氛变为高压力的气氛时，可以保持密闭空间的减压度。将固化性树脂组合物设于胶粘带和透明基板之间的情况下，所涂布的固化性树脂组合物发挥与粘接层同样的作用，因此作为密封构件，也可以使用单面粘接的带或没有粘接层的带。此外，密封构件还可以使用在与夹持于透明基板间的固化性树脂组合物不同的高粘性的固化性树脂组合物中混有间隔物粒子的材料来代替带。此外，用于密封部的固化性树脂组合物为热固性树脂组合物时加热而使其固化，为紫外线固化性树脂组合物时照射紫外线来固化即可。
作为上述减压气氛，将减压气氛的压力设为P1时，较好是满足下式的减压气氛。
10Pa≤P1≤100Pa
这是因为如果P1超过100Pa，则残存于透明层叠体的固化性树脂中的气泡容易变得显著；如果不足10Pa，则减压度高，因此构筑该减压气氛时的负担和时间上的损失增加。此外，还因为如果减压度过高，则对固化性树脂组合物中所含的固化性化合物和其它成分(热聚合引发剂或光聚合引发剂、阻聚剂、光稳定剂等)造成不良影响，因此是不理想的。例如，如果减压度过高，则这些化合物可能会气化。更优选的P1是30～50Pa。
将固化性树脂组合物夹持于一对透明基板间并密封，然后在该减压气氛下夹持固化性树脂组合物规定时间的情况下，自密封固化性树脂组合物时至升高气氛压力为止的减压气氛保持时间没有特别限定。只要可维持密封状态，也可以在固化性树脂组合物刚密封后升高气氛压力。通过在密封后维持减压状态一定时间，固化性树脂组合物在密闭空间内流动，透明基板间的距离变得均匀，即使升高气氛压力也容易维持密闭状态。该减压保持时间可以是数小时以上的较长时间，但从生产效率的角度来看，较好是1小时以内，特别好是10分钟以内。
作为比上述减压气氛高的压力的气氛，较好是大气压。如果是大气压气氛，则不需要用于使固化性树脂组合物固化的特殊设备。但是，并不限定于此，作为比上述减压气氛的压力高的压力，较好是比减压气氛的压力高50kPa以上的压力，特别好是高100kPa以上的压力。
本发明的固化性树脂采用热固性树脂组合物时加热，采用光固化性树脂组合物时照射紫外线即可。或者，可以选择可通过在室温下长时间保持而固化的固化性树脂组合物。另外，除了热聚合引发剂或光聚合引发剂以外，固化性树脂组合物较好是包含量比这些聚合引发剂少的阻聚剂。通过含有阻聚剂，可以改善固化性树脂组合物的稳定性，也可以调整固化后的树脂层的分子量。另外，固化性树脂组合物较好是包含如紫外线吸收剂和自由基捕获剂等光稳定剂。通过含有光稳定剂，可以改善固化后的树脂层的耐光性，是优选的。
作为固化性树脂组合物，特别好是可通过紫外线而固化的光固化性的固化性树脂组合物。例如，热固性树脂组合物包含丙烯酸酯等含丙烯酰氧基的固化性化合物时，为了诱发热聚合引发剂的引发反应，需要加热至例如80℃。与之相对，通过紫外线使包含含丙烯酰氧基的固化性化合物的光固化性的固化性树脂组合物固化时，仅通过照射紫外线即可实现，所以可以节能地使固化性树脂组合物固化。此外，紫外线固化的情况下，温度也不会上升，因此环境负荷小，即使是对热变形的耐受性弱的透明基板也可以使用。室温固化的情况下，需要为了固化而静置例如1天～数天，但紫外线固化的情况下，数分钟～数十分钟就可以使其实质上固化，生产效率高。此外，也可以通过并用紫外线和加热或者紫外线固化后在室温下保持一定时间来完成固化反应。
本发明中，可以使用粘度高的固化性树脂组合物或包含分子量高的固化性化合物的组合物。作为固化性树脂组合物，将固化性树脂组合物的粘度设为Vr时，较好是选择满足下式的粘度的固化性树脂组合物。
0.2Pa·s≤Vr(固化性树脂组合物的25℃的粘度)，且
Vr≤50Pa·s(固化性树脂组合物的40℃的粘度)
为了使25℃的Vr不足0.2Pa·s，需要在固化性树脂组合物中添加一定量以上的低分子量的固化性化合物，因此固化前后的收缩大，固化树脂中残留应变，机械强度低。此外，如果40℃的Vr超过50Pa·s，则透明层叠体的制造过程中固化性树脂组合物的流动性低，因此例如即使在夹持固化性树脂组合物后放置于大气中，因为其流动性不佳，所以固化性树脂组合物扩散至透明基板的间隙整体为止也需要时间。因此，到透明基板的间隙内不存在固化性树脂组合物的空间消失为止需要较长时间，容易导致制造节拍的下降。更好是固化性树脂组合物的25℃的粘度在0.5Pa·s以上，且40℃的粘度在10Pa·s以下。
此外，粘度高的固化性树脂组合物或包含分子量高的固化性化合物的组合物可以使固化树脂中的化学键的数量更少，固化前后的收缩小，因此可以提高固化树脂的机械强度。另一方面，固化性低聚物等分子量大的固化性化合物大多粘性高。因此，从确保机械强度的同时抑制减压层叠时的气泡残留方面来看，较好是使分子量较小的固化性单体溶解于高分子量的固化性低聚物中而调整粘度后使用。作为高分子量的固化性低聚物，较好是分子量1000以上，更好是分子量2000以上。从以上的粘度和分子量的角度来看，制造本发明的透明层叠体时，较好是包含分子量在1000以上的固化性化合物的40℃的粘度在50Pa·s以下的固化性树脂组合物。
此外，固化性树脂组合物较好是固化后形成透明性高的固化树脂的固化性树脂组合物。固化性树脂组合物的固化后的透明性以所得的透明层叠体的雾度值表示，从确保透明层叠体的透明性的角度来看，较好是达到6％以下。另外，为了保持透明层叠体整体的透明性，用于所述密封部的固化性树脂组合物也较好是固化后形成透明性高的固化树脂的固化性树脂组合物。
另一方面，透明层叠体中，将一对透明基板的间隔、即固化树脂层的厚度设为Ts，透明基板中较薄的一块的厚度设为T1，另一块的厚度设为T2时，Ts较好是满足下式。还有，T1和T2也可以是相同的厚度。
T1×0.05≤Ts≤T2×1.5
如果固化树脂层的厚度Ts相对于透明基板中较薄的一块的厚度不足5％，则无法确保作为透明层叠体的强度；如果相对于透明基板中较厚的一块的厚度超过150％，则透明层叠体的厚度没有必要地增大。
透明层叠体中的固化树脂层的厚度确定的情况下，密封部的厚度也等于固化树脂层的厚度Ts。作为密封材料仅使用非压缩性的双面胶粘带时，密封部的厚度与双面胶粘带的厚度大致相等。此外，在双面胶粘带的上表面使用密封部形成用的固化性树脂组合物时(参照图3)，与双面胶粘带和固化性树脂组合物的固化物层的总厚度大致相等。使用由混合有间隔物粒子的固化性树脂组合物形成的密封材料时，密封部的厚度通过间隔物粒子的尺寸来控制。
此外，透明层叠体中，将夹持于一对透明基板的密封部的相对于自垂直方向入射透明基板的光的透射率设为Is，同样夹持于一对透明基板的固化树脂层的透射率设为Ir时，较好是满足下式。
0.9≤Is/Ir≤1.1
通过使密封部的透射率Is相对于固化树脂层的透射率Ir满足上式，透明层叠体整体具有大致相同的透射性，所以可以将透明层叠体整体作为透光体使用。
以下，根据附图对本发明的透明层叠体及其制造方法的优选的实施方式进行说明。
图1～图4中示出表示本发明的透明层叠体的优选的制造步骤的图，图5中示出优选的透明层叠体的制造步骤的流程图。
基于这些图，对本发明的优选的透明层叠体的制造方法进行说明。
首先，准备一对透明基板，并如图1(A)、(B)所示，取出其中的一块透明基板10，沿该透明基板10的4个边缘部粘贴双面胶粘带12，形成密封部(S(步骤)100)。
接着，如图2(A)、(B)所示，在透明基板10的由双面胶粘带12所围成的矩形的区域13涂布(供给)固化性树脂组合物14(S110)。固化性树脂组合物14的涂布量预先设定为通过双面胶粘带12和一对透明基板10、16(参照图3)所密封的空间恰好被固化性树脂组合物14填充的量。涂布方法如下实施：如图2(A)、(B)所示，将透明基板10平放于下平台18，通过沿水平方向移动的给料器20呈线状、带状或点状涂布。该给料器20可通过由一对进给丝杠22、22和与这些进给丝杠22、22垂直的进给丝杠24构成的公知的水平移动机构在所述区域13的整个范围内水平移动。还有，也可以使用模涂装置代替给料器20。
接着，如图3所示，将一对透明基板10、16搬入减压舱26内，通过真空泵28抽吸该减压舱26内的空气。然后，在减压气氛下、例如真空(包括近似真空)气氛下，在将透明基板16通过上平台30的吸盘32、32…吸附保持的状态下，启动汽缸34而使其向在下方待命的透明基板10降下。接着，将一对透明基板10、16介以双面胶粘带12重合(层叠)的同时，在经减压的气氛压力下夹持规定时间(S120)。还有，吸盘32的个数和相对于上平台30的安装位置取决于透明基板16的尺寸等。此外，层叠时的减压度较好是10～100Pa，更好是30～50Pa。
接着，将减压舱26的减压气氛向例如大气开放后(S130)，一对透明基板10、16被大气压压向相互密合的方向。与此同时，残留于密封了的空间的空孔部的体积因该气氛的差压而缩减，所以固化性树脂组合物14流向密闭空间中的减压空间，密闭空间整体被固化性树脂组合物14均匀地填充。然后，使固化性树脂组合物14固化，从而制成本例的透明层叠体。
因此，如果采用通过该制法制成的透明层叠体，一对透明基板10、16通过减压下的气氛被密合，因此成为没有气泡的透明层叠体。此外，由于密闭空间被粘贴于透明基板10的周边部的双面胶粘带12完全地密封，因此在其后的严酷的使用条件下也不易发生自周边部的剥落等，耐久性高。
此外，为了使一对透明基板10、16的粘接性提高，较好是如图3所示在双面胶粘带12的上表面预先涂布密封部形成用的固化性树脂组合物36。通过这样在双面胶粘带12的上表面涂布固化性树脂组合物36，所述的密闭空间的密闭度提高，所以开放至大气压时，可以保持密闭空间的减压度。此外，还可以涂布在与供给于玻璃基板面的固化性树脂组合物不同的高粘性的固化性树脂组合物中混有间隔物粒子的材料来代替双面胶粘带。此外，涂布于双面胶粘带12的上表面的固化性树脂组合物36和密闭空间内的固化性树脂组合物14为光固化性树脂组合物时，使用如图4所示的紫外线照射装置40使固化性树脂组合物14固化。紫外线照射装置40为将来自高压汞灯42、42的紫外线介以反射镜44、44、46、46向被夹持的固化性树脂组合物处于未固化的状态的透明层叠体48的两面整面照射的装置。藉此，可以使涂布于双面胶粘带12的上表面的固化性树脂组合物36和密闭空间内的固化性树脂组合物14同时固化。还有，固化性树脂组合物14为热固性树脂组合物时，加热而使其固化即可。
通过以这样的制造方法制造透明层叠体，作为固化性树脂组合物14，可以使用粘度高的固化性树脂组合物或包含分子量高的固化性化合物的固化性树脂组合物，所以固化时形成强度高的固化树脂，可以获得作为整体机械强度高的透明层叠体。
因此，本发明的透明层叠体与注入低粘度的固化性树脂组合物而制成的以往的透明层叠体相比，即使厚度小，也可以获得足够的透明层叠体的机械强度。此外，即使是通过以往的注入法无法实现的厚度极薄的透明层叠体也可以制造。
固化性树脂组合物14为光固化性的固化性树脂组合物时，仅通过如图4所示照射紫外线即可实现，所以可以节能地使固化性树脂组合物固化。此外，由于温度也不会上升，因此环境负荷小，即使是对热变形的耐受性弱的透明基板也可以使用。
[固化性树脂组合物]
本发明的固化性树脂组合物是通过光或热的作用而固化形成固化树脂的固化性树脂组合物。可以是通过在室温下长时间保持而固化的室温固化性树脂。固化性树脂较好是包含具有聚合性的各种乙烯基的化合物和聚合引发剂的组合物。此外，还可以使用通过乙烯基和巯基的反应而固化的类型的固化性树脂组合物、通过环氧基和藉由光生成阳离子的光阳离子生成剂的组合而固化的类型的固化性树脂组合物、通过结合于硅原子的乙烯基和结合于硅原子的氢原子的反应而固化的类型的固化性树脂组合物等。由于固化速度快，固化树脂的透明性高，特别好是包含至少1种具有选自丙烯酰氧基和甲基丙烯酰氧基的固化性基团的化合物和光聚合引发剂的光固化性的固化性树脂组合物。
作为具有选自丙烯酰氧基和甲基丙烯酰氧基的固化性基团(以下称为(甲基)丙烯酰氧基)的化合物(以下也称(甲基)丙烯酸酯类化合物)，较好是每1分子具有1～6个(甲基)丙烯酰氧基的化合物。为了使固化树脂不变得过硬，特别好是每1分子具有1～3个(甲基)丙烯酰氧基的化合物。(甲基)丙烯酸酯类化合物可以是分子量较低的化合物(以下称为丙烯酸酯类单体)，也可以是具有重复单元的分子量较高的化合物(以下称为(甲基)丙烯酸酯类低聚物)。此外，作为(甲基)丙烯酸酯类化合物，从固化树脂层的耐光性方面来看，较好是使用尽可能不含芳香环的脂肪族类或脂环族类的化合物。
作为(甲基)丙烯酸酯类单体，如果考虑在处理室内的减压下的气氛中向透明基板进行供给的情况，较好是使用具有低至可充分抑制挥发性的程度的蒸气压的化合物。作为(甲基)丙烯酸酯类低聚物，较好是包含聚氨酯链、聚酯链、聚醚链、聚碳酸酯链等具有2个以上的重复单元的链和(甲基)丙烯酰氧基的分子结构的(甲基)丙烯酸酯类低聚物。例如，可以使用被称为氨酯丙烯酸酯低聚物的具有氨酯链(通常还包含聚酯链或聚醚链)和2个以上的(甲基)丙烯酰氧基的(甲基)丙烯酸酯类低聚物。如前所述，低聚物的分子量较好是在1000以上，更好是在2000以上。(甲基)丙烯酸酯类低聚物的粘度过高时，较好是并用丙烯酸酯类单体而使作为(甲基)丙烯酸酯类化合物整体的粘度下降。
此外，作为(甲基)丙烯酸酯类化合物，如果使用分子内具有羟基的化合物，则可以改善与透明基板、特别是玻璃基板的密合性，是优选的。相对于(甲基)丙烯酸酯类化合物整体，具有羟基的(甲基)丙烯酸酯类化合物的含量以重量比计较好是在30％以上，更好是在50％以上。
本发明的固化性树脂组合物较好是包含(甲基)丙烯酸酯类化合物和光聚合引发剂的光固化性的固化性树脂组合物。该光固化性的固化性树脂组合物通过紫外线或可见光的照射而固化，形成固化树脂。作为固化性树脂组合物中的(甲基)丙烯酸酯类化合物，由1种以上的丙烯酸酯类单体、1种以上的(甲基)丙烯酸酯类低聚物或者1种以上的丙烯酸酯类单体和1种以上的(甲基)丙烯酸酯类低聚物形成。特别好是由1种以上的(甲基)丙烯酸酯类低聚物形成，或者由1种以上的(甲基)丙烯酸酯类低聚物和1种以上的丙烯酸酯类单体形成。
通过使用热聚合引发剂代替上述光固化性的固化性树脂组合物中的光聚合引发剂，形成包含(甲基)丙烯酸酯类化合物的热固性的固化性树脂组合物。除了光聚合引发剂和热聚合引发剂以外，这样的光固化性或热固性的固化性树脂组合物中还可以包含阻聚剂、光稳定剂、紫外线吸收剂、抗氧化剂等各种添加剂。这样的固化性树脂组合物的粘度如前所述，较好是25℃的粘度在0.2Pa·s以上，且40℃的粘度在50Pa·s以下。
作为除上述以外的固化性树脂组合物，作为可通过紫外线固化形成良好的树脂层的固化性树脂组合物，可以使用以所含的乙烯基和巯基的摩尔数大致相等的比例包含异氰脲酸三烯丙酯等分子内具有1～6个乙烯基的多烯化合物和2,2'-(1,2-乙二基双氧代)双乙硫醇(triethylene glycol dimercaptan)等分子内具有1～6个巯基的多硫醇化合物且包含光聚合引发剂的光固化性的固化性树脂组合物。此外，还已知包含具有2个以上的环氧基的环氧化合物和光阳离子生成剂的进行光阳离子聚合的固化性树脂组合物，可以在固化物的硬度不过高的范围内使用这样的光固化性的固化性树脂组合物。此外，作为热固性树脂组合物，还可以使用基于分子末端具有乙烯基的硅氧烷化合物和具有氢化硅烷基的化合物的透明的二液性的有机硅树脂。这样的固化性树脂组合物中也同样可以包含阻聚剂、光稳定剂、紫外线吸收剂、抗氧化剂等各种添加剂。
[聚合引发剂]
作为使(甲基)丙烯酸酯类化合物光固化的光聚合引发剂、使多烯化合物和多硫醇化合物反应的光聚合引发剂，可以使用乙酰苯类、缩酮类、苯偶姻或苯偶姻醚类、氧化膦类、二苯酮类、噻吨酮类或醌类等，特别好是苯偶姻异丙醚等苯偶姻醚类或乙酰苯类的光聚合引发剂。此外，作为使环氧化合物固化的光阳离子生成剂，可以使用
Figure GDA00002254353300181
盐类的化合物等。
作为使(甲基)丙烯酸酯类化合物热固化的热聚合引发剂，可以使用过氧化苯甲酰等各种过氧化物或偶氮二异丁腈等偶氮类化合物等。此外，二液型硅氧烷的固化较好是使用铂等催化剂。
[各种添加剂]
作为阻聚剂，可以使用2,5-二叔丁基氢醌等氢醌类或对叔丁基儿茶酚等儿茶酚类、蒽醌类、吩噻嗪类、羟基甲苯类。作为光稳定剂，可以使用苯并三唑类、二苯酮类、水杨酸盐类等紫外线吸收剂或受阻胺等自由基捕获剂。除此之外，作为抗氧化剂，可以使用磷类或硫类的化合物。此外，可以为了形成透明的着色固化树脂层而在固化性树脂组合物中添加各种颜料或染料。由于在减压下的气氛中使用，所述聚合引发剂和这各种添加剂较好是使用分子量较大、减压下的蒸气压小的化合物。
实施例
以下，例示用于确认本发明的有效性而实施的例子。例1和2为实施例，例3为比较例。
[例1]
首先，将厚1mm、宽10mm的双面胶粘带(密封材料)的脱模膜剥离，自长610mm、宽610mm、厚2mm的钠钙玻璃(称为基板A)的玻璃端部沿基板A的4个边部粘合。接着，将100份氨酯丙烯酸酯低聚物(共荣社化学株式会社(共栄社化学社)制UF8001G)和1份苯偶姻异丙醚(聚合引发剂)均匀地混合，将该混合得到的紫外线固化性树脂组合物以约0.3mm的涂布厚度用给料器涂布于所述双面胶粘带的上表面。
另一方面，作为紫外线固化型的固化性树脂组合物(称为组合物P)，使用将70份氨酯丙烯酸酯低聚物(共荣社化学株式会社制UF8001G)、30份二官能甲基丙烯酸酯单体(共荣社化学株式会社制LIGHT-ESTER 14EG)、1份苯偶姻异丙醚均匀地混合而得的组合物，将该组合物置于容器中在开放状态下设置于减压处理室内，通过将处理室内减压至约200Pa·s并保持10分钟来进行脱泡处理。在粘度测定用的容器(博勒飞公司(Brookfield社)制HT-2DB-100)加入约10g组合物P，设置于粘度测定用的保温机，使组合物P的温度为40℃。接着，将安装于粘度计(博勒飞公司制LVDV-Ⅱ+pro)的测定用的转子(博勒飞公司制SC4-31)浸渍于测定容器中的组合物P，以0.3rpm的速度使转子旋转并保持15分钟后，测定组合物P的粘度，结果为16Pa·s。还有，由该结果可知，考虑到树脂的温度依存性，组合物P的温度为25℃时的粘度至少超过0.5Pa·s。
接着，向基板A表面上的以双面胶粘带围成的区域在25℃(室温)下用给料器于多处供给组合物P，使总重量达到380g。接着，将该基板A承载于设置有一对平台的升降装置的真空处理室内的下侧的下平台的上表面。
接着，用吸盘使与基板A使用的基板相同形状且同样厚度的钠钙玻璃板(称为基板B)保持于真空处理室内的升降装置的上侧的上平台的下表面，同时使其在水平方向上达到与基板A相同的位置，在垂直方向上使与基板A的距离保持为10mm。
接着，使真空处理室呈密封状态，排气至真空室内达到约30Pa。然后，通过真空处理室内的升降装置使上下的平台接近，以2kPa的压力压接基板A和基板B，保持1分钟。然后，以约30秒将真空处理室内恢复至大气压，使基板A和基板B介以组合物P密合。
接着，通过升降装置使上下的平台分离，使吸附于上侧的上平台的吸盘的由基板A和基板B形成的层叠体(称为层叠体C)从上侧的上平台剥离。接着，对于层叠体C的外周部的双面胶粘带的上部，隔着玻璃(基板B)自以高压汞灯为光源的光纤光源照射紫外光，使预先涂布于带的通过紫外线而固化的固化性树脂组合物固化。然后，使层叠体C保持水平，静置约1小时。
接着，从层叠体C的面方向均匀地自高压汞灯照射紫外线，使组合物P固化，从而获得夹层玻璃状的透明层叠体(称为层叠体D)。该层叠体D虽然没有以往的采用注入法的制造中所需的气泡除去的步骤，但没有发现残留于固化树脂层中的气泡缺陷等，雾度值也为1％左右，是透明度高的优良制品。还有，雾度值是使用株式会社东洋精机制作所((株)東洋精機製作所)制的HAZE-GARD Ⅱ通过按照ASTM D 1003的测定得到的值。
另外，为了确认层叠体D的强度，进行了落球试验。试验中，将层叠体D设置在JIS R 3205(2005年版)的试验框上，使重4.11kg的铁球从1.5m的高度下落至层叠体D的中央。试验在室温控制在23±2℃的气氛内进行。试验结果为，铁球未贯穿层叠体D。
[例2]
作为紫外线固化型的透明的固化性树脂组合物(称为组合物Q)，使用将70份与例1同样的氨酯丙烯酸酯低聚物(共荣社化学株式会社制UF8001G)、30份单官能丙烯酸酯单体(大赛璐赛泰克株式会社(ダイセル·サイテツク社)制EBECRYL 112)、1份苯偶姻异丙醚均匀地混合而得的组合物，在减压下进行脱泡处理。与例1同样地进行操作，在40℃测定了组合物Q的粘度，结果为9.5Pa·s。还有，由该结果可知，考虑到树脂的温度依存性，组合物Q的温度为25℃时的粘度至少超过0.5Pa·s。
除了固化性树脂组合物使用组合物Q，将减压处理室内保持在30Pa并夹持于一对玻璃基板以外，与例1同样地进行操作，获得层叠体E。通过与例1同样地对层叠体E照射紫外线，获得夹层玻璃状的透明层叠体F。
所得的层叠体F未发现残留的气泡缺陷等，雾度值也为1％左右，是透明度高的优良制品。另外，使用层叠体F以与例1同样的条件实施了落球试验。其结果为，铁球未贯穿。
[例3]
对于与例1相同形状且同样厚度的一对钠钙玻璃基板，将例1中使用的厚1mm、宽10mm的双面胶粘带设置于基板周边部的4边，仅留下1边的双面胶粘带的脱模膜，将一对玻璃基板粘合。
接着，将留有脱模膜的1边的双面胶粘带和玻璃基板之间用螺丝刀挖开2mm左右，试图从该部分同样地注入380g例1中调制的组合物P，但玻璃基板间的下部残留气泡，无法将组合物P密实地注入玻璃基板中。
产业上利用的可能性
本发明的在2块玻璃基板之间形成有树脂制的中间层的透明层叠体因为具有高生产性和优良的品质，所以适合作为建筑物和车辆等的窗玻璃用夹层玻璃。
这里引用2006年12月28日提出申请的日本专利申请2006-354969号的说明书、权利要求书、附图和摘要的所有内容作为本发明说明书的揭示。

Claims (7)

1.透明层叠体的制造方法，该方法是具有一对透明基板和存在于所述一对透明基板间的固化性树脂组合物的固化物的层的透明层叠体的制造方法，其特征在于，在一块透明基板上的周边部形成用于封入固化性树脂组合物的密封部，向透明基板上的以所述密封部围成的区域供给固化性树脂组合物，在减压气氛下在所供给的所述固化性树脂组合物上重叠另一块透明基板，在一对透明基板间夹持固化性树脂组合物并密封，再将夹持有固化性树脂组合物的一对透明基板置于比所述减压气氛的压力高50kPa以上的压力气氛下，在所述压力气氛下使固化性树脂组合物固化；
所述密封部可以保持由该密封部和所述一对透明基板密闭而成的密闭空间的减压度；
所述固化性树脂组合物的25℃的粘度在0.2Pa·s以上，且40℃的粘度在50Pa·s以下。
2.如权利要求1所述的制造方法，其特征在于，所述一对透明基板是具有大致相同的曲率的弯曲基板。
3.如权利要求1或2所述的制造方法，其特征在于，与固化性树脂组合物接触的透明基板表面中的至少一个表面预先以选自硅烷化合物和钛化合物的偶联剂进行了处理。
4.如权利要求1所述的制造方法，其特征在于，在一对透明基板间夹持固化性树脂组合物的减压气氛为10～100Pa的压力气氛。
5.如权利要求1所述的制造方法，其特征在于，使固化性树脂组合物固化的压力气氛为大气压。
6.如权利要求1所述的制造方法，其特征在于，通过加热或紫外线照射使固化性树脂组合物固化。
7.如权利要求1所述的制造方法，其特征在于，固化性树脂组合物为包含至少1种每1分子具有1～3个选自丙烯酰氧基和甲基丙烯酰氧基的固化性基团的化合物和光聚合引发剂的光固化性的固化性树脂组合物。
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