CN115087544A - 用于获得弯曲的层压窗玻璃的方法 - Google Patents

用于获得弯曲的层压窗玻璃的方法 Download PDF

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Publication number
CN115087544A
CN115087544A CN202280002174.4A CN202280002174A CN115087544A CN 115087544 A CN115087544 A CN 115087544A CN 202280002174 A CN202280002174 A CN 202280002174A CN 115087544 A CN115087544 A CN 115087544A
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CN
China
Prior art keywords
layer
glass sheet
enamel
stack
thin
Prior art date
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Pending
Application number
CN202280002174.4A
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English (en)
Inventor
F·弗拉玛里-梅斯波利
J·杰玛特
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Saint Gobain Glass France SAS
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Saint Gobain Glass France SAS
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Filing date
Publication date
Priority claimed from FR2100275A external-priority patent/FR3118768B1/fr
Priority claimed from FR2100402A external-priority patent/FR3118963B1/fr
Priority claimed from FR2101384A external-priority patent/FR3119793B1/fr
Application filed by Saint Gobain Glass France SAS filed Critical Saint Gobain Glass France SAS
Publication of CN115087544A publication Critical patent/CN115087544A/zh
Pending legal-status Critical Current

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    • 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
    • C03C8/10—Frit compositions, i.e. in a powdered or comminuted form containing lead
    • C03C8/12—Frit compositions, i.e. in a powdered or comminuted form containing lead containing titanium or zirconium
    • 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
    • B32B1/00—Layered products having a general shape other than plane
    • B—PERFORMING OPERATIONS; TRANSPORTING
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    • B32B17/061—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 metal
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Abstract

本发明涉及一种用于获得弯曲的层压窗玻璃的方法，其中(a)提供第一玻璃片材(10)，第一玻璃片材在其一个面的至少一部分上涂覆有薄层堆叠体(12)，然后(b)在薄层堆叠体(12)的一部分表面上通过搪瓷组合物的丝网印刷来沉积搪瓷层(14)，该搪瓷组合物以至少0.5%的体积比例包含具有至少20μm的直径的耐火颗粒，但不包含直径大于80µm的颗粒。位于搪瓷层(14)下方的薄层堆叠体(12)随后至少在该弯曲步骤(c)结束时被所述搪瓷层(14)完全溶解。在与附加玻璃片材(20)层压(d)之后，搪瓷层(14)朝向层压中间层(30)。

Description

用于获得弯曲的层压窗玻璃的方法
本发明涉及用于机动交通工具弯曲的层压窗玻璃例如车顶或挡风玻璃的领域，其包括涂覆有薄层堆叠体和搪瓷层的玻璃片材。
层压窗玻璃是其中两个玻璃片材使用层压中间层粘合性结合的窗玻璃。层压中间层尤其允许在破损时保留玻璃碎片，但也提供其它功能性，特别地在抗破坏和防进入或改善声学性质方面。
这些窗玻璃通常包括旨在赋予不同性质的各种类型的涂层。
搪瓷层，通常是黑色和不透明的，通常被沉积在窗玻璃的一部分上，通常呈外围条的形式，旨在隐藏和保护用于将窗玻璃连接和定位在车身窗户开口上的聚合物密封件免受紫外线辐射。搪瓷化区域还隐藏了用于连接内部后视镜和不同连接器和传感器的区域。
在层压窗玻璃中，这些搪瓷层通常被布置在面2上，这些面传统上是从旨在定位在交通工具外部的面开始编号的。因此面2是与层压中间层接触的面。从交通工具外部看，搪瓷层的美观外观对于汽车制备商来说尤为重要。搪瓷通常通过在高于 500℃下烧制包含玻璃料和颜料的组合物来获得。玻璃料由具有低熔点的细玻璃颗粒组成，在烧制热处理的作用下，玻璃粉软化并粘附在玻璃片材上。由此形成通常不透明的矿物层，具有高耐化学性和机械强度，在保持颜料颗粒的同时完美地粘附到玻璃上。烧制步骤通常与玻璃片材的弯曲同时进行。
在制备层压窗玻璃的背景下，窗玻璃的两个玻璃片材通常一起进行弯曲，旨在定位在交通工具内部的玻璃片材通常被布置在承载搪瓷的另一块玻璃片材之上。在其它方法中，每个玻璃片材都是单独弯曲的。在所有情况下，搪瓷必须具有抗粘性质，以防止在弯曲过程中在两个玻璃片材之间或在玻璃片材与弯曲工具之间的任何粘合。为此，通常使用含有铋的搪瓷，即从含有氧化铋的玻璃料中获得的搪瓷。
涂层，通常呈薄层堆叠体的形式，也可以存在于层压窗玻璃的玻璃片材之一上。它尤其可以是可以提供两种类型功能的导电层。首先，当提供电流供应时，导电层可以通过焦耳效应散热。它们这时是加热层，例如可用于除霜或除雾。其次，由于它们反射红外辐射，这些层具有太阳能控制或低辐射性的性质。因此这些层因其提供的热舒适性或节能(通过减少用于供暖或空调的消耗)而受到重视。这些堆叠体通常被布置在层压窗玻璃的面3上，因此也与层压中间层接触。
然而，在某些将在下文中描述的情况下，可以有利的是，将搪瓷层和薄层堆叠体布置在同一玻璃片材上，因此在所讨论的玻璃片材的同一面上，使得这些涂层在层压窗玻璃的内部受到保护。
然而，已经观察到，当涂覆有薄层堆叠体的玻璃片材必须被提供有搪瓷层时，在弯曲时在堆叠体和搪瓷之间可发生不希望的相互作用，特别地导致搪瓷的美学外观下降。特别地已经观察到，特别地当堆叠体包含至少一个氮化物层并且搪瓷包含铋时，在搪瓷内在与堆叠体之间的界面附近产生气泡，导致搪瓷粘附作用显著下降，改变其光学外观(尤其在玻璃一侧，即与搪瓷相反一侧的颜色)并降低其耐化学性，尤其耐酸性。
针对这个问题已经提出了数种解决方案。
可以预先消除在搪瓷层应该被沉积的位置处的薄层堆叠体，例如通过研磨剂，以使搪瓷与玻璃片材直接接触沉积并防止在任何搪瓷层和薄层堆叠体之间的粘合问题。然而，机械磨损会产生可见的划痕，包括在搪瓷层位置。
申请 WO2014/133929 和在其之前的申请 WO0029346 提出了使用特殊玻璃料用于搪瓷的概念，该玻璃料在烧制或预烧期间能够溶解薄层堆叠体以直接附着到玻璃上。然而，这样的搪瓷不具有良好的抗粘性质，导致在弯曲过程中两个玻璃片材彼此粘附。
申请WO2019/106264本身提出通过在堆叠体和包含铋的搪瓷之间添加氧化物层来修改薄层堆叠体。但是，并不总是可以做出这样的改变。
本发明的目的是克服这些问题。
为此，本发明的主题是一种用于获得弯曲的层压窗玻璃，尤其用于机动交通工具的挡风玻璃或车顶的弯曲的层压窗玻璃的方法，包括以下连续步骤：
a. 提供第一玻璃片材，在其一个面的至少一部分上涂覆有薄层堆叠体，
b. 在薄层堆叠体的部分表面上沉积搪瓷层的步骤，该沉积通过使搪瓷组合物丝网印刷来进行，该搪瓷组合物以至少0.5%的体积比例包含具有至少20μm的直径的耐火颗粒，但不包含直径大于80µm的颗粒，
c. 第一玻璃片材的弯曲步骤，位于搪瓷层下方的薄层堆叠体至少在该步骤结束时被所述搪瓷层完全溶解，然后
d. 通过层压中间层将所述第一玻璃片材与附加玻璃片材层压的步骤，使得搪瓷层面对所述中间层。
本发明的另一主题是通过这种方法获得或可获得的弯曲的层压窗玻璃，特别地用于机动交通工具的挡风玻璃或车顶。该窗玻璃包括第一玻璃片材，其在其一个面的至少一部分上涂覆有薄层堆叠体，薄层堆叠体在其表面的一部分上涂覆有搪瓷层，该搪瓷组合物以至少0.5%的体积比例包含直径为至少20μm的耐火颗粒，所述第一玻璃片材通过层压中间层与附加玻璃片材层压，所述搪瓷层朝向所述层压中间层。
本发明还涉及一种搪瓷组合物，其包含基于锌和铋的硼硅酸盐的玻璃料、至少一种颜料和至少0.5体积%的其直径为至少20μm的黑色耐火颗粒。
由搪瓷对薄层堆叠体的溶解允许防止上述相互作用。堆叠体的组成元件溶解在与玻璃片材直接接触的搪瓷层中，搪瓷层至少在弯曲步骤(步骤d)结束时与玻璃片材直接接触。使用耐火颗粒本身允许避免在弯曲期间两个玻璃片材之间的任何粘合。如下文所示，颗粒尺寸的选择允许确保颗粒的均匀沉积，并因此不会发生粘合。
在本文中，薄层堆叠体和搪瓷层统称为“涂层”。
步骤a
第一玻璃片材可以是平坦的或弯曲的。第一玻璃片材在薄层堆叠体和然后搪瓷层的沉积时通常是平坦的，然后在步骤d期间进行弯曲。因此，第一玻璃片材在根据本发明的弯曲的层压窗玻璃中是弯曲的。
第一玻璃片材的玻璃典型地是硅-钠-钙玻璃，但也可以是其它玻璃，例如硼硅酸盐或铝硅酸盐玻璃。第一玻璃片材优选通过浮法，即通过其在于将熔融玻璃倾倒在熔融锡浴上的方法获得。
第一玻璃片材可以由透亮玻璃或有色玻璃制成，优选由有色玻璃制成，例如绿色、灰色或蓝色玻璃制成。为此，第一玻璃片材的化学组成有利地包含氧化铁，其含量为0.5至2重量%。它还可以包含其它着色剂，例如氧化钴、氧化铬、氧化镍、氧化铒或硒。
第一玻璃片材优选地具有包含在0.7至19mm、特别地1至10mm、特别地2至6mm、甚至2至4mm的范围内的厚度。
第一玻璃片材(和附加玻璃片材)的横向尺寸应根据它们旨在被集成到其中的层压窗玻璃的横向尺寸进行调整。第一玻璃片材(和/或附加玻璃片材)优选具有至少1平方米的表面积。
第一玻璃片材优选在玻璃片材的面表面积的至少70%，特别地至少90%，甚至在整个表面积上涂覆有薄层堆叠体。实际上，一些区域可以没有被涂覆以尤其布置允许波通过的通信窗口。
堆叠体优选地在其表面的2至25%，特别地3至20%，甚至5至15%上涂覆有搪瓷层。搪瓷层优选地包括外围带，即自自身闭合的带，其在第一玻璃片材外围的任何点处朝向第一玻璃片材内部延伸一定宽度，该宽度通常可以在典型地1-20 厘米之间变化。
薄层堆叠体优选地与玻璃片材接触。当被沉积时，搪瓷层优选地与薄层堆叠体接触。
在本文中，“接触”意指物理接触。表述“基于”优选意指所讨论的层包含至少50重量%，特别地60重量%，甚至70重量%，甚至80重量%或90重量%的所考虑材料的事实。该层甚至可以基本上由这种材料组成或由这种材料组成。“基本上由...组成”应理解为表示该层可以包含对其性质没有影响的杂质。术语“氧化物”或“氮化物”不必然意味着氧化物或氮化物是化学计量的。实际上，它们可以是亚化学计量的、超化学计量的或化学计量的。
堆叠体优选地包括至少一个基于氮化物的层。氮化物特别是至少一种选自铝、硅、锆、钛中的元素的氮化物。它可以包括至少两种或三种这些元素的氮化物，例如氮化硅锆或氮化硅铝。优选地，基于氮化物的层是基于氮化硅的层，更特别地是基本上由氮化硅组成的层。当氮化硅层通过阴极溅射进行沉积时，它通常包含铝，因为通常的是用铝掺杂硅靶以加速沉积速率。
基于氮化物的层优选具有在2至100nm、特别地5至80nm范围内的物理厚度。
基于氮化物的层通常用于许多薄层堆叠体，因为在它们防止在堆叠体中存在的其它层(特别是将在下面描述的功能层)被氧化的意义上它们具有有利的阻挡性质。
堆叠体优选地包括至少一个功能层，特别是导电功能层。功能层优选地包括在两个薄介电层之间，其中至少一个是基于氮化物的层。其它可能的介电层例如是氧化物层或氮氧化物层。
至少一个导电功能层有利地选自：
- 金属层，特别是银或铌层，甚至金层，和
-透明导电氧化物层，特别地选自氧化铟锡、掺杂的氧化锡(例如掺杂氟或锑)、掺杂的氧化锌(例如掺杂铝或镓)。
这些层因其低辐射性而特别受重视，这为玻璃提供优异的隔热性质。在装备陆地交通工具，特别地机动交通工具、铁路交通工具，或空中或海上交通工具的窗玻璃中，低辐射窗玻璃允许在炎热的天气中向外反射部分太阳辐射，从而限制所述交通工具乘客舱的加热，并必要时降低空调费用。相反，在寒冷的天气里，这些窗玻璃允许将热量保留在乘客舱内，并因此减少所需的加热能量。这在装配建筑物的窗玻璃的情况下同样如此。
根据一种优选的实施方案，薄层堆叠体包括至少一个银层，特别地一个、两个、三个甚至四个银层。银层的物理厚度或适当时银层厚度的总和优选为2-50nm，特别是3-40nm。
根据另一种优选的实施方案，薄层堆叠体包括至少一个氧化铟和氧化锡层。其物理厚度优选在30-200nm之间，特别地在40-150nm之间。
为了在弯曲步骤期间保护该或每个导电薄层(无论它是金属的还是基于透明导电氧化物的)，这些层中的每一个优选地被至少两个介电层包围。介电层优选基于至少一种选自硅、铝、钛、锌、锆和锡中的元素的氧化物、氮化物和/或氮氧化物。
薄层堆叠体的至少一部分可以通过各种已知技术，例如化学气相沉积(CVD)，或通过阴极溅射，特别地磁场辅助的阴极溅射(磁控管方法)进行沉积。
薄层堆叠体优选地通过阴极溅射，特别地磁场辅助的阴极溅射进行沉积。在这种方法中，等离子体在高真空中在包含待沉积化学元素的靶的附近产生。通过轰击目标，等离子体的活性物质撕下所述元素，该元素沉积在玻璃片材上，形成所需的薄层。当该层由从靶上撕下的元素与等离子体中包含的气体之间的化学反应产生的材料构成时，该方法称为“反应性”方法。这种方法的主要优点在于可以通过使玻璃片材在不同靶(通常在同一设备中)下连续运行，在同一条生产线上沉积非常复杂的层堆叠体。
上述堆叠体具有用于提供加热功能(除霜、除雾)和/或隔热功能的导电和红外反射性质。
当薄层堆叠体旨在提供加热功能时，必须提供电流供应。它尤其可以是通过丝网印刷在玻璃片材的两个相反边缘处的薄层堆叠体上沉积的银浆条。
步骤 b
在本文中，将在步骤b期间用于沉积湿搪瓷层的液体组合物称为“搪瓷组合物”。术语“搪瓷层”用于描述该方法每个阶段的层，无论湿层(预烧之前，必要时在干燥之前)还是最终层(在烧制后)。
在步骤b期间，搪瓷层优选地由包含至少一种颜料、至少一种玻璃料和耐火颗粒的搪瓷组合物进行沉积。与搪瓷层一样，搪瓷组合物优选不包含氧化铅。
搪瓷组合物通常还包含有机介质，旨在促进组合物施用在基材上以及其与基材的暂时粘附，并且在搪瓷的预烧或烧制期间被消除。介质典型地包含溶剂、稀释剂、油和/或树脂。
玻璃料能够溶解下面的层堆叠体。优选地，玻璃料基于硼硅酸锌铋。为了使其对层堆叠体更具“侵略性”，铋和/或硼的含量优选高于通常使用的玻璃料的含量。
颜料优选包含一种或多种选自铬、铜、铁、锰、钴和镍的氧化物的氧化物。例如，它可以是铜和/或铁铬酸盐。
“耐火颗粒”是指在弯曲过程中其形态不受到明显影响的颗粒。这些颗粒必须远高于在弯曲过程中所经历的温度的熔化或软化温度，并且也不再应该被玻璃料溶解。耐火颗粒尤其基于金属氧化物或金属。金属氧化物特别地简单的氧化物，如，例如氧化铝、氧化锆或氧化钛，或复杂的氧化物，例如高熔点玻璃料或无机颜料(后者特别地被称为“复合无机彩色颜料”或CICP )，尤其黑色无机颜料。
已经观察到，搪瓷组合物必须包含足够比例的“大”耐火颗粒(因此尺寸，也称为直径，为至少20 µm)，以防止玻璃片材在弯曲过程中彼此粘附，或者玻璃片材与弯曲工具粘附。由于它们的尺寸，大的耐火颗粒在弯曲过程中会形成一种形态，其中颗粒形成峰，熔融或软化的玻璃料聚集在谷中。这种 20 µm 或更大的尺寸比玻璃料和常规使用的颜料大得多。
尺寸(或直径)为20μm及以上的耐火颗粒的体积比例优选通过激光粒度测量法测定。该比例为至少0.5%，优选至少1%，特别地至少2%，甚至至少3%。
优选地，搪瓷组合物以上述体积比例包含其直径为至少30μm，特别地至少40μm，甚至至少50μm的耐火颗粒。
另一种表征搪瓷组成和容易检测大颗粒存在的方式在于用Hegman量规(或研磨细度规)测量颗粒的细度。根据该方法，用Hegman量规测量的搪瓷组合物的细度在20-80μm之间，特别地在40-60μm之间。
搪瓷组合物不应该包含直径大于 80 µm 的颗粒(难熔或非难熔)，以便允许通过丝网印刷的沉积。这种颗粒的存在可以通过激光粒度测量法或用Hegman量规进行确定。
耐火颗粒优选是基于氧化锆的。基于氧化锆的颗粒是指包含至少80重量%，特别地85重量%的氧化锆(ZrO2)的颗粒。氧化锆优选进行稳定化，特别地用钇进行稳定化。它还可以包含烧结助剂添加剂，特别地选自Al2O3、TiO2、ZnO、SiO2和它们的混合物。
优选地，基于氧化锆的颗粒的化学组成以如下重量含量范围包含以下成分，特别地由它们组成：
- ZrO2：83-97%
-Y2O3：2-8%
-Al2O3：0-3%
-黑色颜料：0-6%，特别地1-6%。
基于氧化锆的颗粒优选进行煅烧，特别地在1100-1500℃之间的温度下进行煅烧。
基于氧化锆的颗粒优选具有通过激光粒度测量法测定确定的体积粒度分布，使得D10 为至少 20 μm，特别地在 30-45μm 之间，D50 在 40-52μm 之间，并且 D90为最多65µm，特别地在 55-65µm 之间。
耐火颗粒，尤其基于氧化锆，优选是黑色的。特别地，反射亮度L*优选小于3，甚至优选小于1。比色坐标a*和b*优选各自小于0.5，特别地小于0.1。比色参数根据标准 ISO7724 (D65-10°) 确定。为此目的，颗粒，特别地基于氧化锆的颗粒，可包含黑色颜料，其含量典型地为1-6重量%。
耐火颗粒，特别地黑色耐火颗粒的平均球形度优选大于0.60，尤其大于0.70，甚至大于0.80，甚至大于0.85。颗粒的球形度对应于最小Féret直径与最大Féret直径之间的比率。耐火颗粒的平均圆度优选大于0.6，特别地0.7，甚至0.8或0.9。平均球形度(或圆度)对应于 50 至 200 个颗粒的球形度(或圆度)的算术平均值。圆度对应于 4*A/π.Lf²，Lf 是最大的Féret直径，A 是颗粒的投影面积。这些不同的参数，特别地Féret直径，尤其通过动态图像分析进行测量，例如使用由Horiba公司销售的Camsizer XT粒子分析仪进行测量。
已经能够观察到，使用没有过多凹凸不平的黑色颗粒和/或球形颗粒允许改善在烧制后搪瓷的美感，特别地通过减少在强照明下从面1反射中可见的雾度。
搪瓷层的沉积通过丝网印刷进行。为此，将丝网印刷丝网放置在玻璃片材上，该丝网包括网孔，网孔中一些被堵塞，然后将搪瓷组合物沉积在丝网上，然后施用刮刀以迫使搪瓷组合物在丝网的网孔未堵塞的区域中穿过丝网，以形成湿搪瓷层。为了保证大的耐火颗粒的均匀沉积，丝网的网孔开口优选为至少40μm，特别地至少60μm，甚至至少70μm。网孔开口太小会捕获颗粒并阻止其均匀沉积，而网孔开口太大会导致搪瓷厚度太高，这有会在机械上削弱玻璃的风险。网孔开口优选为至多100μm，特别地至多80μm。
湿搪瓷层的厚度优选在15-40μm之间，特别地在20-30μm之间。
优选地，步骤b之后立即进行干燥步骤，旨在消除在搪瓷组合物中包含的溶剂中至少一部分。这种干燥通常在120至180℃的温度下进行。
步骤 c
弯曲尤其可以在通常为 550 至 650℃的温度下通过重力(玻璃在其自身重量下变形)或通过压制进行实施。
根据第一种实施方案，两个玻璃片材(第一玻璃片材和附加玻璃片材)分别弯曲。在这种情况下，重要的是避免在第一玻璃片材和弯曲工具之间的任何粘合。
根据第二种实施方案，第一玻璃片材和附加玻璃片材一起进行弯曲，搪瓷层朝向所述附加玻璃片材。在这种情况下，重要的是要避免两个玻璃片材之间的任何粘合。玻璃片材可以通过在它们之间放置中间粉末(确保几十微米的间隙，通常为20至50μm)来保持分开。中间粉末为例如基于碳酸钙和/或碳酸镁。在弯曲过程中，内部玻璃片材(旨在位于乘客舱内)通常放置在外部玻璃片材上方。因此，在弯曲步骤期间，将附加玻璃片材放置在第一玻璃片材上方。
优选地，在步骤d之后，搪瓷层是不透明的，具有黑色调。在玻璃一侧的反射中测量的其亮度L*优选小于5。如上所指出，它有利地在第一玻璃片材的外围形成条带。搪瓷层由此能够隐藏和保护密封件、连接元件或传感器免受紫外线辐射。
如果在下述预烧之后搪瓷层还没有完全溶解该薄层堆叠体，这这种溶解在弯曲过程中实现，从而完成搪瓷烧制。
薄层堆叠体的完全溶解可以通过电子显微镜进行观察。电测量，特别地平方电阻，也允许确定堆叠体的溶解。
任选的预烧步骤 (b1)
该方法优选地包括，在步骤b)和步骤c)之间，预烧搪瓷层的步骤b1)，在该步骤期间，位于搪瓷层下方的薄层堆叠体至少部分地被所述搪瓷层溶解。
该步骤在前面描述第二种实施方案中特别有用，其中所述玻璃片材一起进行弯曲。
预烧步骤优选在150至800℃，特别地500至700℃的温度下进行。
这样的预烧允许消除有机介质，或者通常任何任选存在于搪瓷层中的有机成分。
在预烧期间，薄层堆叠体至少部分地被搪瓷层溶解。根据所使用的温度和搪瓷或堆叠体的类型，堆叠体甚至可以在预烧过程中被搪瓷层完全溶解。或者，它可以在预烧过程中仅部分溶解，然后在弯曲过程(步骤c)中完全溶解。
步骤 d
层压步骤可以通过在高压釜中处理来进行，例如在110至160℃的温度和10至15巴的压力下。在高压釜处理之前，夹在玻璃片材和层压中间层之间的空气可以通过压延或施加负压来消除。
如上所述，附加片材优选地是层压窗玻璃的内部片材，即位于窗玻璃凹侧的片材，旨在定位在交通工具的乘客舱内。因此，涂层被布置在层压窗玻璃的面2上。
附加玻璃片材可由钠-钙-硅玻璃或硼硅酸盐或铝硅酸盐玻璃制成。它可以由透亮或有色玻璃制成。它的厚度优选地在0.5-4mm之间，特别地在1-3mm之间。
根据一种优选的实施方案，附加玻璃片材具有0.5-1.2mm的厚度。附加玻璃片材特别由钠铝硅酸盐玻璃制成，优选进行化学强化。附加玻璃片材优选地是层压窗玻璃的内片材。本发明对于这种类型的配置特别有用，对于这种配置，难以在面3上布置薄层堆叠体。化学强化(也称为“离子交换”)在于使玻璃表面与熔融钾盐(例如硝酸钾)接触，使得通过用较大离子半径的离子(在这种情况下为钾离子)交换玻璃的离子(在这种情况下为钠离子)来增强玻璃表面。这种离子交换允许在玻璃表面上并且在一定厚度上形成压缩应力。优选地，表面应力为至少300MPa，特别地400甚至500MPa，并且至多700MPa，并且压缩区的厚度为至少20μm，典型地在20-50μm之间。应力分布可以使用配备有 Babinet 补偿器的偏光显微镜以已知方式进行确定。化学淬火步骤优选在380至550℃的温度下进行为30分钟至3小时的持续时间。化学强化优选在弯曲步骤之后但在层压步骤之前进行。获得的窗玻璃优选是机动交通工具的挡风玻璃，特别地加热挡风玻璃。
根据另一个优选的实施方案，附加玻璃片材在与朝向层压中间层的面相反的面上(优选面4，附加片材是内部片材)承载附加薄层堆叠体，特别地具有低辐射性的堆叠体，其包含透明导电氧化物，特别地氧化铟锡(ITO)。本发明对于这种类型的配置也特别有用，对于这种配置，将薄层堆叠体布置在同一玻璃片材的两个面上(面3和4)上是很棘手的。在这种实施方案中，层压中间层和/或附加玻璃片材优选是着色的，其中带有涂层的玻璃片材可以由透亮玻璃制成。获得的窗玻璃优选是机动交通工具的车顶。
作为后一个优选的实施方案的示例，可以提及弯曲的层压车顶，该车顶从交通工具外部起包括在面2上涂覆有薄层堆叠体的透明玻璃片材(该薄层堆叠体包括至少一个银层然后是搪瓷层)、由有色 PVB 制成的层压中间层和由有色玻璃制成的附加玻璃片材，在面 4 上承载有低辐射性的薄层堆叠体，特别地基于 ITO。
层压中间层优选包含至少一层聚乙烯醇缩醛，特别地聚乙烯醇缩丁醛(PVB)。
如果需要，层压中间层可以被着色或不着色，以调节窗玻璃的光学或热性质。
层压中间层可以有利地具有吸声性质以便吸收空气来源的或固体来源的声音。为此，它可以特别由三个聚合物片材组成，包括两个围绕内部聚合物片材的“外部”PVB片材，任选地由PVB制成，其硬度低于外部片材的硬度。
层压中间层还可以具有隔热性质，特别地红外辐射反射的性质。为此，它可以包括具有低辐射性的薄层涂层，例如包含薄银层的涂层或具有不同折射率的介电层交替的涂层，其被沉积在由两个外部PVB片材围绕的内部PET片材上。
层压中间层的厚度通常在0.3-1.5mm的范围内，特别地为0.5-1mm。层压中间层在窗玻璃边缘的厚度可以小于在窗玻璃中心的厚度，以防止在使用抬头显示系统(HUD)的情况下形成双重图像。
实施例
以下示例性实施例通过结合图1以非限制性方式说明本发明。
[图1]示意性地说明了根据本发明的方法的一个实施方案。它显示了一部分玻璃片材和沉积在玻璃片材上在其周边附近的元件的示意性横截面。各种元件显然没有按比例表示，以便能够将它们可视化。
在步骤a)中提供涂覆有薄层堆叠体12的第一玻璃片材10，然后堆叠体12的一部分涂覆有搪瓷层14，特别地通过丝网印刷(步骤b)进行。
然后该组件经历预烧(步骤b1)，在所显示的情况下，这引起堆叠体12被搪瓷14部分溶解。
然后将附加玻璃片材20放置在第一玻璃片材10上，在这里附加玻璃片材被提供有附加薄层堆叠体22，然后将该组件弯曲(步骤c)。所示视图仅为玻璃片材端部的视图，此处未显示弯曲。该图说明了，在弯曲结束时，搪瓷14已经完全溶解了在下面的薄层堆叠体12的事实。
在步骤d中，用薄层堆叠体12和搪瓷层14涂覆的第一玻璃片材10和用附加堆叠体22涂覆的附加玻璃片材20借助于层压中间层30进行组装。此处的该图在这里以分解视图的形式表示每个单独的元件。
由实施例实施的方法对应于图1的实施方案。
2.1 毫米厚的玻璃片材(其预先通过阴极溅射用薄层堆叠体进行涂覆，该薄层堆叠体包括三个由氧化锌层、氮化硅层和NiCr阻挡剂保护的银层)已通过丝网印刷用湿厚度为 25 µm的搪瓷层涂覆。
搪瓷组合物包含尺寸大于 20 µm 的难熔氧化物大颗粒。
使用了两种类型的颗粒：下表中表示为A的颗粒，具有为白颜色和不规则形状，和在下表中表示为B的颗粒，其基于氧化锆，具有黑颜色，并且呈现出比颗粒A更圆的形状。颗粒B是由Saint-Gobain Zirpro以标号ColorYZe G Black销售的黑色氧化锆颗粒，在1300℃的温度下进行煅烧。
颗粒B具有以下化学组成(按重量计)：ZrO2：89.6%，Y2O3：5.26%，Al2O3：1.05%，黑色颜料：4.1%。体积粒度分布如下：D10=40μm，D50=49μm，D90=60μm。
下面的表1对于每个测试指示了这些颗粒的体积比例，以“体积%”表示。
根据实施例，搪瓷层的沉积使用网孔开口为71μm(丝网1)或49μm(丝网2)的丝网进行实施。
然后将搪瓷干燥(150℃，1-2分钟)，然后在大约650℃-680℃下预烧。
在与由硅-钠-钙玻璃制成的附加玻璃片材(在面4上被提供有包括ITO层的堆叠体)配对后，将该组件在超过600℃下弯曲350至500秒。
烧制后，通过测量在反射中的亮度L*(光源D65，参考观察者10°)来评估美学外观，更特别是从面1看到的黑色。小于或等于6.0，优选小于5.0的值被认为是可接受的。关于它们，通过目视观察定性评估模糊度(从玻璃的面1)和粘合。
对于粘合，使用0到5的等级，其中0分对应于无缺陷，1分对应于在角上的有限搪瓷转移，2分对应于在角和边上的搪瓷转移，3分对应于在角上的粘合，4分对应于在角和边上的粘合，5分对应于完全粘合。超过3分是不可接受的。
[表1]
Figure 866781DEST_PATH_IMAGE001
。
比较例C0表明，不存在大的耐火颗粒导致完全粘合。在比较例C1的情况下，添加了耐火材料粒子，但量过少，不能充分地减少粘合。在实施例C2的情况下，尺寸大于80μm的耐火颗粒的存在不允许通过丝网印刷沉积搪瓷层。
添加耐火材料颗粒A(实施例1和2)允许减少这种粘合，当大颗粒的比例和丝网印刷丝网的网孔尺寸较大时更是如此，但会产生轻微的模糊。
在实施例3和4的情况下，黑色的且比颗粒A更球形的颗粒B使得可以在降低模糊度的同时实现不粘合。

Claims (15)

1.一种用于获得弯曲的层压窗玻璃，尤其用于机动交通工具的挡风玻璃或车顶的弯曲的层压窗玻璃的方法，包括以下连续步骤：
a. 提供第一玻璃片材(10)，在其一个面的至少一部分上涂覆有薄层堆叠体(12)，
b. 在薄层堆叠体(12)的一部分表面上沉积搪瓷层(14)的步骤，该沉积通过使搪瓷组合物的丝网印刷来进行，该搪瓷组合物以至少0.5%的体积比例包含具有至少20μm的直径的耐火颗粒，但不包含直径大于80µm的颗粒，
c. 第一玻璃片材(10)的弯曲步骤，位于搪瓷层(14)下方的薄层堆叠体(12)至少在该步骤结束时被所述搪瓷层(14)完全溶解，然后
d. 通过层压中间层(30)将所述第一玻璃片材(10)与附加玻璃片材(20)层压的步骤，使得搪瓷层(14)朝向所述中间层(30)。
2.根据权利要求1所述的方法，使得所述薄层堆叠体(12)包括至少一个功能层，特别地导电功能层。
3.根据前一项权利要求所述的方法，其中所述导电功能层选自金属层，特别地银层或铌层，和透明导电氧化物层，特别地选自氧化铟锡、掺杂氧化锡和掺杂氧化锌的氧化物的层。
4.根据前述权利要求中任一项所述的方法，使得在步骤d之后，所述搪瓷层(14)是不透明的，具有黑色色调，并且在所述第一玻璃片材(10)的外围形成条带。
5.根据前述权利要求中任一项所述的方法，其中所述耐火颗粒基于金属氧化物或金属。
6.根据前一项权利要求所述的方法，其中所述金属氧化物是简单的氧化物，例如铝、钛或甚至锆的氧化物，或复杂的氧化物，例如具有高熔点的玻璃料或无机颜料。
7.根据前一项权利要求所述的方法，其中所述耐火颗粒基于氧化锆。
8.根据前述权利要求中任一项所述的方法，其中，所述耐火颗粒是黑色的。
9.根据前述权利要求中任一项所述的方法，其中所述耐火颗粒的平均球形度大于0.60，尤其大于0.70。
10.根据前述权利要求中任一项所述的方法，其中，所述搪瓷层(14)的沉积通过丝网印刷使用具有至少40μm的网孔开口的丝网印刷丝网来进行。
11.根据前述权利要求中任一项所述的方法，使得：
-所述方法在步骤b)和步骤c)之间包括搪瓷层(14)的预烧步骤b1)，在其期间，位于搪瓷层(14)下方的薄层堆叠体(12)至少部分地被所述搪瓷层(14)溶解，和
-在步骤c)中，第一玻璃片材(10)和附加玻璃片材(20)一起进行弯曲，搪瓷层(14)朝向所述附加玻璃片材(20)。
12.根据前述权利要求中任一项所述的方法，其中，所述附加玻璃片材(20)具有0.5-1.2mm的厚度，特别地由化学增强的铝硅酸钠玻璃制成。
13.根据前述权利要求中任一项所述的方法，其中，所述附加玻璃片材(20)在与朝向所述层压中间层(30)的面相反的面上承载附加薄层堆叠体(22)，特别地包含透明导电氧化物的具有低辐射性的堆叠体。
14.能够通过前述权利要求任一项的方法获得的弯曲层压窗玻璃，特别地用于机动交通工具的挡风玻璃或车顶，其包括第一玻璃片材(10)，其在其一个表面的至少一部分上涂覆有薄层堆叠体(12)，所述第一玻璃片材(10)在其一部分表面上涂覆有搪瓷层(14)，该搪瓷层(14)以至少0.5%的体积比例包含直径为至少20μm的耐火颗粒，所述第一玻璃片材(10)通过层压中间层(30)与附加玻璃片材(20)进行层压，所述搪瓷层(14)朝向所述层压中间层(30)。
15.用于实施根据权利要求8所述的方法的搪瓷组合物，其包含基于铋和锌的硼硅酸盐的玻璃料、至少一种颜料和至少0.5体积％的直径为至少20μm的黑色耐火颗粒，但不包括直径大于80µm的颗粒。
CN202280002174.4A 2021-01-13 2022-01-11 用于获得弯曲的层压窗玻璃的方法 Pending CN115087544A (zh)

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EP2832704A1 (en) * 2012-03-29 2015-02-04 Mitsuboshi Belting Ltd. Ceramic color paste, ceramic color, glass having ceramic color, and manufacturing method thereof
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