CN110719898A - 低发射率玻璃 - Google Patents
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Abstract
本发明涉及低发射率玻璃,其包括:玻璃衬底;形成在所述玻璃衬底上的第一电介质层;形成在所述第一电介质层上的金属层;形成在所述金属层上的吸收层;形成在所述吸收层上的第二电介质层;以及形成在所述第二电介质层上并且含有Zr的涂层,由此提供了具有良好并且优异的处理和长期储存性质的低发射率玻璃。
Description
技术领域
本发明涉及具有优异的耐久性、处理和长期储存性质的低发射率玻璃。
背景技术
通过在玻璃表面上特别地涂覆,低发射率玻璃在夏季反射太阳辐射热并且在冬季保持由室内加热器产生的红外线,由此增加建筑物的节能作用。
此类低发射率玻璃主要以两种方式制造。一种是其中在玻璃制造过程期间将半导体前体均匀地应用于热玻璃带上,使得前体通过玻璃热被分解和涂覆的方法。另一种是其中通过在真空室中溅射金属靶进行涂覆的方法。
在前者的情况下,通常通过涂覆SnO2:F材料来进行制造,并且由于相对稳定的氧化物的在高温下的沉积和使用,涂膜的涂覆程度具有非常牢固的性质但低发射率性质。在后者的情况下,通过以膜的形式涂覆金属来进行制造,并且考虑价格、颜色和低发射率性质,主要使用银作为金属。此外,由于银具有低耐久性的性质,以玻璃衬底/电介质/银/电介质/保护层的形式制造低发射率玻璃。然而,由于相对不稳定的银的物理沉积和使用,涂层是不牢固的,并且因此耐久性是差的。
因此,出于改善低发射率玻璃的涂层的目的,已经提出了各种方法。例如,在第1,080,245号欧洲注册专利的情况中,将Zn氧化物与Sn一起添加以用作电介质,将Ti层用作银的保护层,并且将附加层用作顶部保护层。在第5,834,103号美国注册专利的情况中,将Zn氧化物用作电介质,将Ti用作银的保护层,并且将Si氮化物用作顶部保护层。在第6,010,602号美国注册专利的情况中,将Zn-Sn氧化物用作电介质,将Ti用作银的保护层,并且将TiO2用作顶部保护层。如以上所述,已经进行了使用各种材料和各种结构的发明以改善基于金属的低发射率玻璃的耐久性。然而,在具有高的温度和湿度的雨季的地区中,耐久性,尤其耐湿性是不好的。因此,需要研究以解决当长时间储存在高温度和高湿度的地区中时由于涂膜的劣化的诸如光点和变色缺陷的问题。
发明内容
技术问题
本发明的方面提供了具有除了耐久性以外的优异的处理性质(例如耐寒性和耐酸性)和长期储存性质的低发射率玻璃。
技术方案
根据本发明的方面,提供了低发射率玻璃,其包括玻璃衬底、形成在所述玻璃衬底上的第一电介质层、形成在所述第一电介质层上的金属层、形成在所述金属层上的吸收层、形成在所述吸收层上的第二电介质层、以及形成在所述第二电介质层上的包含Zr的涂层。
有益效果
与使用TiOxNy的常规低发射率玻璃相比,本发明的低发射率玻璃在处理、长期储存和机械耐久性方面是优异的,并且具有的优点在于沉积速率是优异的并且稳定的溅射是可能的。
附图简述
本文所附的以下附图通过实例例示出本发明的优选实施方案,并且用于使本发明的技术构思连同以下给出的本发明的详细描述一起能够被进一步理解,并且因此本发明不应仅用此类附图中的内容来解释。
图1是示出本发明的单个低发射率玻璃的层压结构的视图;
图2的(a)至(c)是示出图1的单个低发射率玻璃中的具体的层压结构实例的视图;
图3是示出本发明的多片低发射率玻璃的层压结构的视图;以及
图4的(a)至(c)是示出图3的多片低发射率玻璃中的具体的层压结构实例的视图。
附图中使用的参考数字如下:
10:玻璃衬底
20:第一电介质层
21:第二电介质层
22:电介质层
20a、21a、22a:主电介质层
20b、21b、22b:次电介质层
30:金属层
40、40a、40b:吸收层
50:涂层
用于进行本发明的最佳模式
在下文,将参考附图描述本发明的优选实施方案。然而,本发明不限于本文描述的实施方案。在附图中,为了清楚起见,可以放大层和区域的厚度。在整个说明书中,相同的参考数字是指相同的元件。此外,在以下描述本发明时,当确定详细描述可能不必要地使本发明的要点模糊时,将省略对相关的已知功能或配置的详细描述。
在下文,将更详细地描述本发明以促进对本发明的理解。
应理解,在本发明的说明书和权利要求中使用的词语或术语不应被解释为限于具有在通常使用的字典中定义的含义。还应理解,基于发明人可以适当地定义词语或术语的含义以最好地解释本发明的原则,词语或术语应被解释为具有与其在相关领域的背景中和本发明的技术思想中的含义一致的含义。
图1是示出本发明的单个低发射率玻璃的层压结构的视图。
参考图1,本发明的低发射率玻璃包括玻璃衬底10、形成在玻璃衬底10上的第一电介质层20、形成在第一电介质层20上的金属层30、形成在金属层30上的吸收层40、形成在吸收层40上的第二电介质层21、以及形成在第二电介质层21上的包含Zr的涂层50。
玻璃衬底10用作低发射率玻璃的基体衬底。常规玻璃,例如钠钙玻璃、低铁玻璃、绿盘玻璃或用于建筑物或汽车的蓝盘玻璃可以用作玻璃衬底10。此外,根据使用的目的,可以自由地使用具有2mm至12mm的厚度的玻璃。例如,可以使用具有5mm或6mm的厚度的透明的钠钙玻璃。
第一电介质层20形成在玻璃衬底10上,并且用于在热处理(例如加固和弯曲)期间阻挡递送至金属层30的氧或离子。第一电介质层20包括主电介质层20a,并且可以选择性地具有形成在主电介质层20a的上部或下部上的次电介质层20b。根据本发明的一个实施方案,如图2的(a)和(b)中所示,次电介质层20b可以形成在主电介质层20a的上部上,即,在主电介质层20a与金属层30之间。
主电介质层20a可以由含有选自Al、B、Ti、Nb、Sn和Mo中的一种或多种元素的基于Si的氮化物或氮氧化物形成,并且次电介质层20b可以由含有选自Sn、Nb、Al、Sb、Mo、Cr、Ti和Ni中的一种或多种元素的基于Zn的氧化物形成。
根据本发明的一个实施方案,主电介质层20a可以是SiAlNx,其中x是1.3≤x≤1.5。如果x超出以上数值范围,则沉积速率可能由于过量的氮(N2)而变差。次电介质层20b可以是ZnAlOx,其中x是0.5≤x≤3。如果x超出以上数值范围,则沉积速率可能由于过量的氧(O2)而变差。
主电介质层20a和次电介质层20b中的每一个的厚度可以独立地是5nm至50nm。具体地,主电介质层20a的厚度可以是30nm至50nm,并且次电介质层20b的厚度可以是5nm至20nm。如果主电介质层20a的厚度小于30nm或者次电介质层20b的厚度小于5nm,则耐久性可能变差。如果主电介质层20a的厚度大于50nm或者次电介质层20b的厚度大于20nm,则可能降低透射率。
根据本发明的一个实施方案,如图2的(b)和(c)中所示,在第一电介质层20与金属层30之间可以进一步包括吸收层40a。
金属层30选择性地反射太阳辐射以用于实现低辐射的同时提供高屏蔽性能。具有良好导电性的金属可以用作金属层30,并且可以使用选自Ag、Cu、Au、Al和Pt中的一种或多种。根据本发明的实施方案,用作金属层30的金属可以是银(Ag)。
金属层30的厚度可以是5nm至25nm。如果金属层30的厚度小于5nm,则不能适当地进行金属层30的形成,使得不能充分地实现低辐射性能。如果大于25nm,则透射率变差并且反射率增加,使得开放感可能变差。
参考图1和图2,吸收层40、40a或40b是与金属层30接触的层,并且用于改善金属层30与电介质层之间的粘附性,以防止在热处理(例如加固和弯曲)期间从玻璃扩散的Na+以及空气中的O2的移动,以帮助金属的融化,以即使在高热处理温度下也能使金属层30的性能稳定,并且最后吸收渗入金属层30的O2以帮助保持低发射率性质。
对于吸收层40、40a或40b,可以使用选自Ni、Cr和Ni-Cr合金中的一种。当使用Ni-Cr合金时,合金可以具有,例如75wt%至85wt%的Ni和15wt%至25wt%的Cr的组成。对于根据本发明的实施方案的吸收层40、40a或40b,可以使用Ni-Cr合金。
吸收层40、40a或40b的厚度可以是0.1nm至10nm。当吸收层40、40a或40b的厚度小于0.1nm时,耐久性可能变差,并且在热处理和弯曲过程之后,涂膜的雾度可能增加。当大于10nm时,在热处理和弯曲过程之后,透射率可能降低并且涂膜的雾度可能增加。
参考图1和图2,第二电介质层21用于在热处理(例如加固和弯曲)期间阻挡递送至金属层30的氧或离子。如第一电介质层20,第二电介质层21包括主电介质层21a,并且可以选择性地具有形成在主电介质层21a的上部或下部上的次电介质层21b。根据本发明的一个实施方案,如图2的(b)中所示,次电介质层21b可以形成在主电介质层21a的下部上,即,在主电介质层21a与吸收层40b之间。
主电介质层21a可以由含有选自Al、B、Ti、Nb、Sn和Mo中的一种或多种元素的基于Si的氮化物或氮氧化物形成,并且次电介质层21b可以由含有选自Sn、Nb、Al、Sb、Mo、Cr、Ti和Ni中的一种或多种元素的基于Zn的氧化物形成。根据本发明的一个实施方案,主电介质层21a可以是SiAlNx,其中x是1.3≤x≤1.5。如果x超出以上数值范围,则沉积速率可能由于过量的氮(N2)而变差。次电介质层21b可以是ZnAlOx,其中x是0.5≤x≤3。如果x超出以上数值范围,则沉积速率可能由于过量的氧(O2)而变差。
主电介质层21a和次电介质层21b的厚度可以独立地是5nm至70nm。具体地,主电介质层21a的厚度可以是35nm至70nm,并且次电介质层21b的厚度可以是5nm至20nm。如果主电介质层21a的厚度小于35nm或者次电介质层21b的厚度小于5nm,则耐久性可能变差。如果主电介质层21a的厚度大于70nm或者次电介质层21b的厚度大于20nm,则可能降低透射率。
包含Zr的涂层50用于保护根据本发明的低发射率玻璃的表面,并且具有高机械强度、低表面粗糙度和高透射率的材料可以用作涂层50。
包含Zr的涂层50可以包含Zr,或者Zr和选自Si、Ti、Al、Cu、Fe、Ni、Pb和Nb中的至少一种的复合金属,并且涂层50可以包括Zr或Zr复合金属的氮化物、氧化物和氮氧化物。具体地,涂层50可以包含选自ZrNx(例如,0.5≤x≤2)、SiZrNx(例如,0.5≤x≤2)、SiZrTiOx(例如,0.5≤x≤3)、SiZrAlNx(例如,0.5≤x≤2)和ZrTiOxNy(例如,0.5≤x≤3,0.5≤y≤2)中的至少一种。在此,当x或y超出所述数值范围时,沉积速率和密度可能降低。
涂层50的厚度可以优选地是1nm至20nm。如果涂层50的厚度小于1nm,则耐久性可能变差。如果大于20nm,则透射率可能变差,或者可能引起雾度。
图3是示出本发明的多重(例如,双重或三重)低发射率玻璃的层压结构的视图。
参考图3,本发明的低发射率玻璃可以还包括在图1的层压结构中的吸收层40与第二电介质层21之间的至少一种多层结构,所述多层结构在其中依次包括电介质层22、金属层30和吸收层40。当在如图1中所示的单个层压结构中包括如以上描述的一个多层结构时,其被称为双重低发射率玻璃,并且当进一步包括两个多层结构时,其被称为三重低发射率玻璃。
如第一电介质层20和第二电介质层21,电介质层22用于在热处理(例如加固和弯曲)期间阻挡递送至金属层30的氧或离子。参考图4的(a),如第一电介质层20和第二电介质层21,电介质层22包括主电介质层22a,并且可以选择性地具有形成在主电介质层22a的上部或下部上的次电介质层22b。
如图4的(b)和(c)中所示,多层结构中的至少一个可以进一步包括在电介质层22与金属层30之间的至少吸收层40a。
在下文,将参考实施例详细地描述本发明。
然而,以下实施例仅是本发明的例示,并且本发明不受到以下实施例限制。
[实施例]
实施例1
使用磁控管溅射涂布机,制造具有形成在6mm透明玻璃衬底上的多层涂膜的低发射率玻璃,所述多层涂膜具有以下表1中显示的组成和厚度。
在氮气/氩气(氮气比例:40体积%)气氛下涂覆第一电介质层(SiAlNx,x=1.3至1.5),并且在氩气100%气氛下涂覆吸收层(NiCr合金),以及在氩气100%气氛下涂覆金属层(Ag)。此后,在氩气100%气氛下,在金属层(Ag)上涂覆吸收层(NiCr合金),在氮气/氩气(氮气比例:40体积%)气氛下涂覆第二电介质层(SiAlNx,x=1.3至1.5),并且使用金属靶在氮气/氩气(氮气比例:40体积%)气氛下涂覆ZrN层作为涂层以制造低发射率玻璃。
实施例2
以与实施例1中相同的方式制造低发射率玻璃,但使用金属靶在氮气100%气氛下涂覆ZrN层作为涂层。
[表1]
[比较例]
比较例1
以与实施例1中相同的方式制造低发射率玻璃,但使用陶瓷靶在氮气/氩气(氮气比例:40体积%)气氛下涂覆TiOxNy(x:y=3:1)层作为涂层。
比较例2
以与实施例1中相同的方式制造低发射率玻璃,但使用陶瓷靶在氧气/氩气(氧气比例:50体积%)气氛下涂覆ZrO层作为涂层。
[表2]
[实验性实施例]
根据以下方法测量在实施例和比较例中的每一个中获得的低发射率玻璃的物理性质,结果显示在以下表3中。
耐湿性
将涂覆有在实施例和比较例中的每一个中制造的低发射率玻璃的一个样品制备成100×100mm的尺寸,并且然后放置在恒温和恒湿室(相对湿度80±10%,温度30±2℃)中。在固化24小时后,以1天(24小时)的间隔取出样品,并且用布从其中去除水,以确定样品是否满足针孔(Φ)的尺寸和数量以及以下1)至3)。
1)4.0mm≤Φ不允许多于一个
2)2.0mm≤Φ不允许多于三个
3)不允许正面的小针孔
耐刮擦性
1)一般
将涂覆有在实施例和比较例中的每一个中制造的低发射率玻璃的一个样品制备成300×100mm的尺寸,并且然后将样品放置在膜厚测定仪1720中,其涂覆表面朝上以便与刷子接触。将蒸馏水应用于样品的涂覆表面上,并且然后操作装置(刷子往返200次)。完成后,从样品中去除水并目视确认以记录等级。此时,等级评估标准如下。
-1级:无划痕
-2级:5个或更少的宽度小于0.1mm的细划痕
-3级:6个或更少的宽度小于0.1mm的细划痕
-4级:2个或更少的宽度大于0.1mm的宽划痕
-5级:3个至5个宽度大于0.1mm的宽划痕
-6级:6个或更多的宽度大于0.1mm的宽划痕,以及发生宽度小于1.0mm的涂膜剥离
-7级:发生超过1.0mm的涂膜玻璃。
2)石英(严苛的)
将涂覆有在实施例和比较例中的每一个中制造的低发射率玻璃的一个样品制备成400×100mm的尺寸,并且然后将样品放置在埃里克森刷子测试仪(Erichsen BrushTester)中,其涂覆表面朝上以便与刷子接触。将石英粉末溶液应用于样品的涂覆表面上,并且然后操作装置(刷子往返50次)。完成后,从样品中去除水并目视确认以记录等级。此时,等级评估标准与1)一般评估标准中的那些相同。
耐寒性
将涂覆有在实施例和比较例中的每一个中制造的低发射率玻璃的一个样品制备成100×300mm的尺寸,并且然后使用移液管将2.5g的制备的人工汗试剂(含有2.5g的NaCl(99%)、L-组氨酸盐酸盐·1水合物(99%)、1.25g的磷酸二氢钠·12水合物(98%)以及500ml的DI水)滴样品的涂覆表面上。此后,将样品放置在恒温和恒湿室(相对湿度80±10%,温度30±2℃)中。放置样品后,以1小时间隔在距样品50cm的距离处检查涂膜的状态。
耐酸性
将涂覆有在实施例和比较例中的每一个中制造的低发射率玻璃的一个样品制备成50×100mm的尺寸,并且然后将1N HCl溶液填充至实验塑料容器中的1/3点。此后,将样品放置在其中。在室温下以1小时间隔用蒸馏水清洗样品的涂覆表面,并且然后用布从其中去除水。用裸眼以50cm的距离在视觉上确认样品的涂覆表面的状态。
克利夫兰(Cleveland)
将涂覆有在实施例和比较例中的每一个中制造的低发射率玻璃的一个样品制备成400×600mm的尺寸,并且然后安装样品使得涂覆有低发射率玻璃的样品的表面面向水分凝结测试仪(其可以将浴的温度保持在60±1℃)的内部。此后,使用夹具固定样品。4小时后,以1小时间隔检查涂覆表面的针孔和损坏。
[表3]
Claims (13)
1.低发射率玻璃,包括:
玻璃衬底;
形成在所述玻璃衬底上的第一电介质层;
形成在所述第一电介质层上的金属层;
形成在所述金属层上的吸收层;
形成在所述吸收层上的第二电介质层;以及
形成在所述第二电介质层上的包含Zr的涂层。
2.如权利要求1所述的低发射率玻璃,其中所述涂层还包含Zr、或者Zr和选自Si、Ti、Al、Cu、Fe、Ni、Pb和Nb中的至少一种的复合金属。
3.如权利要求1或2所述的低发射率玻璃,其中所述涂层包含Zr或Zr复合金属的氮化物、氧化物和氮氧化物。
4.如权利要求1所述的低发射率玻璃,其中所述涂层是选自ZrNx(0.5≤x≤2)、SiZrNx(0.5≤x≤2)、SiZrTiOx(0.5≤x≤3)、SiZrAlNx(0.5≤x≤2)和ZrTiOxNy(0.5≤x≤3,0.5≤y≤2)中的至少一种。
5.如权利要求1所述的低发射率玻璃,其中所述涂层的厚度是1nm至20nm。
6.如权利要求1所述的低发射率玻璃,其中所述第一电介质层和所述第二电介质层中的至少一个还包括主电介质层并且选择性地包括形成在所述主电介质层的上部或下部上的至少一个次电介质层。
7.如权利要求6所述的低发射率玻璃,还包括在所述第一电介质层与所述金属层之间的吸收层。
8.如权利要求1至6中任一项所述的低发射率玻璃,包括在所述吸收层与所述第二电介质层之间的至少一个多层结构,所述多层结构在其中依次包括电介质层、金属层和吸收层。
9.如权利要求8所述的低发射率玻璃,其中所述电介质层还包括主电介质层并且选择性地包括形成在所述主电介质层的上部或下部上的至少一个次电介质层。
10.如权利要求9所述的低发射率玻璃,其中所述至少一个多层结构还包括在所述电介质层与所述金属层之间的至少一个吸收层。
11.如权利要求6或9所述的低发射率玻璃,其中所述次电介质层由含有选自Sn、Nb、Al、Sb、Mo、Cr、Ti和Ni中的一种或多种元素的基于Zn的氧化物形成,并且所述主电介质层由含有选自Al、B、Ti、Nb、Sn和Mo中的一种或多种元素的基于Si的氮化物或氮氧化物形成。
12.如权利要求1所述的低发射率玻璃,其中所述金属层是选自Ag、Cu、Au、Al和Pt中的一种或多种。
13.如权利要求1所述的低发射率玻璃,其中所述吸收层是与所述金属层接触的层并且包含Ni、Cr或Ni-Cr合金。
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US20140186636A1 (en) * | 2011-03-03 | 2014-07-03 | Guardian Industries Corp. | Barrier layers comprising ni-inclusive ternary alloys, coated articles including barrier layers, and methods of making the same |
US20140072784A1 (en) * | 2012-09-07 | 2014-03-13 | Anton Dietrich | Coated article with low-e coating having absorbing layers for low film side reflectance and low visible transmission |
US20160185660A1 (en) * | 2013-08-16 | 2016-06-30 | Guardian Industries Corp. | Coated article with low-e coating having low visible transmission |
US20160298384A1 (en) * | 2013-12-12 | 2016-10-13 | Lg Hausys, Ltd. | Low-emissivity coating film, method for manufacturing same, and functional construction material for window and doors including same |
Also Published As
Publication number | Publication date |
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KR20190011384A (ko) | 2019-02-07 |
EP3659984A4 (en) | 2020-07-22 |
KR102082424B1 (ko) | 2020-02-27 |
EP3659984A2 (en) | 2020-06-03 |
WO2019022383A3 (ko) | 2019-04-11 |
WO2019022383A2 (ko) | 2019-01-31 |
US20200189972A1 (en) | 2020-06-18 |
JP2020522454A (ja) | 2020-07-30 |
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