CN1044358C - 溅射镀膜的玻璃制品 - Google Patents

溅射镀膜的玻璃制品 Download PDF

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CN1044358C
CN1044358C CN93105250A CN93105250A CN1044358C CN 1044358 C CN1044358 C CN 1044358C CN 93105250 A CN93105250 A CN 93105250A CN 93105250 A CN93105250 A CN 93105250A CN 1044358 C CN1044358 C CN 1044358C
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K·W·哈蒂格
P·J·灵格尔
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    • C03C17/00—Surface treatment of glass, not in the form of fibres or filaments, by coating
    • C03C17/34—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions
    • C03C17/36—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions at least one coating being a metal
    • C03C17/3602—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions at least one coating being a metal the metal being present as a layer
    • C03C17/3618—Coatings of type glass/inorganic compound/other inorganic layers, at least one layer being metallic
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    • C03C17/3652—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions at least one coating being a metal the metal being present as a layer the coating stack containing at least one sacrificial layer to protect the metal from oxidation
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    • C03C17/00—Surface treatment of glass, not in the form of fibres or filaments, by coating
    • C03C17/34—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions
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    • C03C17/3657—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions at least one coating being a metal the metal being present as a layer the multilayer coating having optical properties
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    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
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    • C23C14/18—Metallic material, boron or silicon on other inorganic substrates
    • C23C14/185—Metallic material, boron or silicon on other inorganic substrates by cathodic sputtering
    • G—PHYSICS
    • G02—OPTICS
    • G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
    • G02B5/00—Optical elements other than lenses
    • G02B5/20—Filters
    • G02B5/28—Interference filters
    • G02B5/281—Interference filters designed for the infrared light
    • G02B5/282—Interference filters designed for the infrared light reflecting for infrared and transparent for visible light, e.g. heat reflectors, laser protection
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    • C03C2217/00—Coatings on glass
    • C03C2217/70—Properties of coatings
    • C03C2217/78—Coatings specially designed to be durable, e.g. scratch-resistant
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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    • Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
    • Y10T428/00—Stock material or miscellaneous articles
    • Y10T428/12—All metal or with adjacent metals
    • Y10T428/12493—Composite; i.e., plural, adjacent, spatially distinct metal components [e.g., layers, joint, etc.]
    • Y10T428/12535—Composite; i.e., plural, adjacent, spatially distinct metal components [e.g., layers, joint, etc.] with additional, spatially distinct nonmetal component
    • Y10T428/12542—More than one such component
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    • Y10T428/12493—Composite; i.e., plural, adjacent, spatially distinct metal components [e.g., layers, joint, etc.]
    • Y10T428/12535—Composite; i.e., plural, adjacent, spatially distinct metal components [e.g., layers, joint, etc.] with additional, spatially distinct nonmetal component
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    • Y10T428/12535—Composite; i.e., plural, adjacent, spatially distinct metal components [e.g., layers, joint, etc.] with additional, spatially distinct nonmetal component
    • Y10T428/12597—Noncrystalline silica or noncrystalline plural-oxide component [e.g., glass, etc.]

Abstract

一种高性能和耐久的低辐射率玻璃，它的可见光透射率约为80%或更高，半球辐射率(Eh)约为0.13或更小，正常辐射率(En)约为0.10或更小，该玻璃通过在玻璃基底上溅镀一个多层体系而形成，该多层体系包括一个Si3N4底镀层和一个顶镀层，至少一个银层和至少两个镍或镍合金的夹层，镍合金最好是镍铬合金，铬以铬的氮化物的形式存在。

Description

溅射镀膜的玻璃制品
本发明涉及溅射镀膜的玻璃及其制造方法。更具体地说，本发明涉及溅射镀膜的玻璃及制造它们的一些独特的方法，这些玻璃具有高的可见光透射率和优良的反射红外能的特性，可以作为建筑玻璃使用。
对于诸如用“浮法”制得的建筑用平板玻璃，在玻璃上形成控制日光的涂层的两种较重要的方法是高温喷涂法和磁溅镀膜法。迄今为止的溅射镀膜法的缺点是镀层常常容易被擦掉(即，缺乏“耐久性”)和在构成建筑用多层窗玻璃中用的聚合密封剂常常侵蚀镀层。这又破坏了各层之间的密封，使得有害的凝结物会累积在各层之间。另一方面，溅射镀膜具有历史性的优点，与大多数高温喷涂相比，它能达到低的辐射率和高的可见光透射率的性能。这两个性质或许在某些建筑玻璃中属于最需要达到的性质之列。
“辐射率”和“透射率”这些术语是本技术中众所周知的，本文中使用的是它们为人熟知的含义。例如，“透射率”一词在本文中是指日光透射率，它由可见光透射率、红外能透射率和紫外光透射率构成。因此，总的日光透射率常常表示成这些数值的重均值。关于这些透射率，本文中报道的可见光透射率是用标准的施照体(即光源)C技术在380-720纳米下测得的；红外透射率在800-2100纳米；紫外透射率在300-400纳米；总日光透射率为300-2100纳米。但是，对于辐射率来说，则采用如下所述的特定的红外范围(即，2,500-40,000纳米)。
可见光透射率可以用已知的常规方法测定。例如，使用分光光度计，如Beckman5240(Beckman科学仪器公司)，得到在各波长下透射率的光谱曲线。然后用ASTME-308“用CIE系统计算物体颜色的方法”(ASTM标准年鉴，卷14.02)计算可见光透射率。如果愿意，可以采用数目少于规定值的波长。另一种测定可见光透射率的方法是使用一种分光计，例如太平洋科学公司制造的市售的Spectragard分光光度计。此种装置直接测定和显示出可见光透射率。
“辐射率”(E)是指在给定波长下光的吸收和反射的量度或特征。它常用以下公式表示：
E-=1-反射率膜
就用于建筑而言，辐射率数值在红外光谱的所谓“中间范围”、有时也称作“远区”，即，约2,500-40,000纳米，变得相当重要。本文中用的“辐射率”一词，是指在1991年推荐的ASTM标准规定的这一红外范围内测得的辐射率数值，此标准是主要玻璃制造商协会提议用来测定红外能以便计算辐射强度，题目为“用辐射测量法测定和计算建筑用平板玻璃产品辐射强度的试验方法”。此标准及其规定在本文中引用作为参考。在此标准中，辐射率分成两部分：半球辐射率(Eh)和正常辐射率(En)。
用于测定这些辐射率数值的实际的数据积累过程是常规的，可以用例如带“VW”附件的Beckman4260型分光光度计(Beckman科学仪器公司)完成。这种分光光度计测量出反射率随波长的变化，由此出发，利用本文引用作为参考的上述1991准荐ASTM标准计算辐射率。
本文使用的另一名词是“薄膜电阻”。薄膜电阻(Rs)是本技术中众所周知的名词，本文中按照它的为人熟知的含义使用。一般来说，此名词是指在玻璃基底上的任何平方面积的层状体系对通过该层状体系的电流的电阻(欧姆)。薄膜电阻是该层反射红外能好坏的标志。因此常与辐射率一起作为这一特性的量度，在很多建筑玻璃中也很重要。“薄膜电阻”可方便地用一个四探针欧姆计测定，例如一个可调配的四点电阻率探针和一个Magnetron仪器公司装置(M-800型，由Signatone公司(Santa Clara California)制造)。
如上所述，对于很多建筑用途而言，希望辐射率和Rs值尽可能低，以便使玻璃窗反射掉射在玻璃上的相当大数量的红外能。一般来说，“低辐射率”玻璃是指半球辐射率(Eh)少于约0.16、正常辐射率(En)低于约0.12的那些玻璃。最好是Eh约为0.13或更小，En约为0.10或更小。与此同时，薄膜电阻(Rs)最好小于约10.5欧姆/平方面积。这类玻璃若要商业上合用，通常要求透过尽可能多的可见光，用测定透射率的施照体C技术在约2毫米-6毫米厚的玻璃中得到的透射率经常为约76％或更高。在这一方面，对于厚度在2-6毫米之间的玻璃，可见光透射率应当至少约为78％或更高。可见光透射率为约80％或更高则更好，最好是大于约80％。
用磁溅镀膜法在平板玻璃板上镀上多层金属和/或金属氧化物或氯化物来形成建筑玻璃的方法是众所周知的，而且已经尝试和报道了大量的已知金属(例如金、银等)、氧化物和氮化物的排列与组合。这种方法可以在多靶区内使用平面靶或管形靶，或者二者的组合，以达到理想的结果，本技术中已知的可用于本发明的优选装置的实例是Airco公司销售的磁溅镀膜机。美国专利4,356,073和4,422,916分别公开了这种市售装置。这些专利公开的内容在本文中引用作为参考。
具体地说，已知用上述的Airco溅射镀膜机制造具有层状体系的建筑玻璃，该层状体系从玻璃(例如标准浮法玻璃)向外顺序如下：
Si3N4/Ni∶Cr/Ag/Ni∶Cr/Si3N4其中实际上已经发现Ni∶Cr合金的Ni/Cr重量比为80/20(镍铬合金)，其中的两个镍铬合金层据报道为7厚，Ag层规定只有约70厚(除了声明银层可以厚100左右的以外)，Si3N4各层相对较厚(例如，底镀层为320，顶镀层约为450)。实际上，因为太薄的缘故(即70左右)，已发现银(Ag)层实质上是多少有些半连续的。
图1(下面更全面地解释)示意说明上面提到的用来制造这种已知Airco产品的一种典型的Airco溅射镀膜机。参看图1，区1、2、4和5由管形硅(Si)靶)(“t”)构成，溅射是在100％的N2 气氛中进行，区3通常使用平面靶“p”，用来形成三个中间层，即Ni∶Cr/Ag/Ni∶Cr。使用100％的氩气氛。在溅射镀膜工艺中是过去认为、而且在此之前一直认为N2在溅射镀膜期间对银有不利影响，因此要小心地保持第3区中基本上不含N2。
虽然这种镀层实现了良好的“耐久性”(即，镀层耐刮伤、耐磨和化学上稳定)，因而与高温喷涂相比达到了这一特性的重要指标，但是实际上已经发现，它的其它特性不合乎通常对低辐射率建筑玻璃所要求的红外反射率和可见光透射率特性的标准。例如，对于约3毫米厚的玻璃，可见光透射率(施照体C)常常只约为76％，Eh约为0.20-0.22,En约为0.14-0.17。这两种辐射率均相当高。另外，薄膜电阻(Rs)经测量为相当高的15.8欧姆/平方面积(更合乎要求的数值是10.5左右或更小)。因此，虽然耐久性显著改善了，而且这些镀层也与常规的密封剂相容(从而克服了多层窗工艺中的这一问题，该工艺通常要求“边缘空白”，现在不再要求)，但是日光控制质量比很多现代建筑用途所要求的最佳质量差。
除了这种Airco多层体系外，在专利和科学文献中还报道了用含银和/或Ni∶Cr的其它镀膜作为红外反射和其它控光用途的多层体系。例如，在美国专利3,682,528和4,799,745(以及其中讨论和/或引用的先有技术)中公开了Fabry-Perot滤光片和其它的先有工艺镀层和技术。还可以参见在许多专利中制成的介电的金属夹层结构，例如美国专利4,179,181,3,698,946,3,978,273,3,902,997和3,889,026,它们只是其中的几个。虽然其它这些镀层是已知的或是已有报道，但是据信在本发明之前，这些先有技术中没有一个提到或者实现了能用溅射镀膜法大量生产，同时生产出不仅在耐久性方面接近或等于高温喷涂产品、而且还具有优良的控制日光品质的建筑玻璃。
还应该指出，虽然基本的Airco设备和基本操作方法已经相当合乎要求，但是它的生产能力低。低生产能力的原因与假设在溅射期间银必须与N2隔绝有关，我们已发现这一假设对于我们的发明不适用。
根据以上所述，显然在本技术中需要一种溅射镀膜的多层体系，它在耐久性方面与高温喷涂产品接近或相当，但是具有最佳的控制日光的特性，从而克服了高温喷涂法通常带有的问题。本文中使用的名词“耐久的”或“耐久性”是根据它们在本技术中众所周知的含义使用，在这一方面它们反映出与高温喷涂法接近或相当的对机械及化学破坏作用的阻力。由上述显然可见，本技术需要一种用磁溅镀膜法产生的镀膜，它在改进透射率和辐射率的同时，最好也改进在上述Airco方法下得到的这些镀层的薄膜电阻，并且还提高这一已知方法的生产能力。
本发明的目的是满足以上需要和本技术中的其它需要，一旦提供了以下的公开内容，对于熟练的技术人员这将是显而易见的。
一般来说，本发明通过提供一种溅射镀膜的玻璃制品满足了本技术中的上述需要，该制品由一个玻璃基底和它上面的一个多层体系构成，该多层体系由玻璃向外包含有：一个Si3N4底镀层，第一层镍或镍合金，一层银，第二层镍或镍合金，和一个Si3N4顶镀层，其中当玻璃基底的厚度约为2-6毫米时，带镀层的玻璃最好是可见光透射率至少约78％(施照体C)，正常辐射率(En)小于约0.12，半球透射率(Eh)小于约0.16。
在某些特别优选的实施方案中，这种多层体系是“耐久的”，可见光透射率如上所述至少为约80％或更大，最好是大于80％。在另一个优选的实施方案中，辐射率数值中Eh约为0.13或更小，En约为0.10或更小。最好是Eh约为0.12-0.13，En约为0.09-0.10，在这些实施方案中，优选的薄膜电阻范围是10.5欧姆/平方面积或更小，最好是约9-10欧姆/平方面积。
在本发明的另一些优选的实施方案中，多层体系由上述五层构成，不含其它层。在其它的优选实施方案中，多层体系可以增加不干扰或破坏本发明镀层基本质量的其它已知镀层。在某些情形下，这些附加的镀层实际上可以提高镀层的基本质量。例如，本发明考虑的这种其它层状体系之一主要由七层体系构成，它是用一个镍基层(例如镍-铬)将银层分成两层而形成的，一于是该多层体系由玻璃向外现在主要包括：
Si3N4/Ni∶Cr/Ag/Ni∶Cr/Ag/Ni∶Cr/Si3N4与上述的五层体系相比，据信这种七层体系一般具有多少更好些的耐久性和抗擦伤特性，同时红外反射率更高。
有时，附加层可以包括任选的顶镀层以增大抗擦伤性，或者包括底镀层以改善粘着力等等。但是，在实施本发明时，最优选的一体系是上述的五层体系和七层体系。
在实施本发明中已经发现，在优选的实施例中，为了达到所要求的最佳辐射率和透射率特性，各层的厚度对于获得理想的最终结果相当重要。在这一方面，与已知的上述Airco五层体系相比，发现将银层的厚度增加超过Airco规定值70约为20％-30％很重要，以便在银是单层时确保它是基本上连续的银层，而在一般情况下则确保具有适当的红外反射率。因此，对于本发明，不采用规定的Airco70银层，而是采用总厚度约为90-105、最好是约95-105的银层。
对于本发明的具有单个Ag层的五层体系，银层厚度以约95为佳。在银层被夹在中间的镍基层分成两层的那些实施方案中，两层的总厚度应该约为90-105，最好是每层约为50。在这方面，应该指出在50时银层变得多少有些不连续。尽管这一情况在Airco体系中是一个问题，但是在实施本发明中不产生不利的影响。
使用的镍基层最好是在Airco体系中使用的同样的Ni∶Cr(80/20)镍铬合金。但是，不采用Airco规定的10(或更大)的厚度，Ni∶Cr层常保持厚度小于约7(例如6或更小，或减小约15-20％)。
按照与对总银层采用的类似方式，本发明的各个Si3N4层的厚度比Airco体系的各层厚度增加。在优选的的实施方案中，厚度增加与银层增加处在同一量级，例如约20％或更大。因此，在优选的实施方案中，不用Airco规定的厚度分别约为320和450的Si3N4底镀层和顶镀层(底层比顶层稍薄)，在实施本发明时，Si3N4底镀层厚度以至少约为400、顶镀层厚度以至少约540为宜。最好是底层约为400-425，顶层约为540-575。这些Si3N4层的作用主要是为了防反射、颜色控制、耐化学物质、耐擦伤和耐磨。
多层窗玻璃在建筑中普遍使用。已经发现本发明的多层体系与制造这些窗玻璃使用的常规密封剂完全相容，从而将本技术中的这一问题克服到Airco多层体系所达到的同样程度。因此，在本发明的优选的实施方案中，不需要“边缘空白”。
与以前在本技术中所持的看法完全相反的是本发明的以下发现，即，对于本文所考虑的某些优选的多层体系，不仅不需要在溅射期间将银与N2隔离，而且在N2环境下将银和镍基层一起溅射会有好处。在这方面，银的性能没有显著损失。这本身又导致出乎意料地发现，如果镍基层中含有铬，而且铬在溅射期间转化成氮化物，则透射性质令人惊奇地提高。因此，在本发明的某些优选的实施方案中，Ni基靶是Ni∶Cr合金，Cr在溅射期间在与银同一个溅射区内转化成(至少是部分地)Cr的氮化物。正如已提到的，已经发现这样作会使最终产品的可见光透射率显著提高。另外，由于在溅射银的同一区内生成这种氮化物，所以降低了花费并提高了生产能力。
与Airco方法相比，生产能力的提高和成本的降低是按以下方式进行的：在Airco方法(及其它方法)中，Si溅射既难又慢，因为施加在靶(例如Airco方法中的管形靶)上的功率由于使用100％N2气氛而必须增加，经常要增加到设备的极限。在银必须不在含N2环境中溅射的假设下，而且如果想将Cr转化成氮化物，则Ni∶Cr靶就不得不敢在另一个区内，从而增加了额外的费用。另一种作法是将这些靶在与Si相同的含N2区内溅射，但是由于减少了可供使用的Si靶数目而降低了产量。在实施本发明中发现的在溅射期间形成铬的氮化物有利和N2对Ag无不利影响这一事实，排除了对以上的昂贵和对生产不利的替代方案的需要，因为现在两个N2∶Cr靶可以处在和银靶相同的区内，而且现在可以在Ar/N2气氛中进行溅射，而不是象以前认为的必须在纯氩气氛中。在这一方面，优选的实施方案中使用50/50体积的Ar/N2，但是可以采用在0％-75％Ar和100％-25％N2之间的更广的范围。
如上所述，Airco方法提到在100％N2气氛中溅射Si。虽然目前这是根据本发明进行Si溅射阶段的一种方法，但是也已经发现，在某些情况下(例如小装置少量生产)可以在溅射Si期间向N2中加氩，以便以已知的方式提高Si的溅射速度，同时仍形成合乎要求数量的Si3N4。
基于以上考虑，本发明通过提供一种制造上述制品的新方法进一步满足了上述需要，该方法包括在同一区内溅镀Ni∶Cr/Ag/Ni∶Cr靶，同时使用含有足够N2的气氛产生Cr的氮化物。这种气氛以含有约0％-75％体积的Ar和约100％-25％的N2为宜。最好是约50％体积的N2和50％的Ar，在某些实施方案中，底镀层和顶镀层在100％的N2气氛中进行溅镀，而在另一些实施方案中可以使用含3％-50％体积Ar和N2以提高生产能力。
现在将根据一些实施方案并参照附图对本发明作出说明，其中：
图1是可以用来实施本发明的Airco设备(在实施上述先有技术时其用法不同)的示意图。
图2是先有技术Airco多层体系的部分侧视截面图。
图3是本发明的一个实施方案的部分侧视截面图。
图4是本发明另一实施方案的部分侧视截面图。
参看图1，该图画出了一个常规的磁溅镀膜机，例如上面提到的Airco装置。在实施本发明时，最好使用5个区(1-5)。(当玻璃G沿箭头A方向前进时，各层顺序地镀于其上。)区1包括6个管形硅(Si)靶t1-6(例如，掺杂3-5％重量Al的Si以提高电导率)。区2包括另外6个同样材料的管形靶t7-12。以类似的方式，区4和5分别各包括同样材料的另外6个管形靶t19-24和t25-30。
中间区3最好由3个平面靶p1-3(即，标号分别为31、16和33)构成，用来制成示于图3的五层体系，或是由5-6个靶(即，管形或平面靶)构成，用来制备示于图4的七层体系。图示的三平面靶系统当然也能用来制造示于图2的先有技术Airco多层体系。对于图4的7层体系，区3中靶的排列是熟练技术人员能够选择的。为方便起见没有画出。假设在区1-2和4-5中六个靶位的可利用性与这类装置的典型情况相同，采用的一种得到所需相对厚度的三个镍基层(例如镍铬合金)的方法是使用靶(31)和(33)[即，p1和p2]作为镍基靶，并且用一系列在p1和p3之间的靶代替靶(16)[即p2]，其中t13是银，t14是镍基靶，而t15和t15均为银靶。
在操作时，区1-5用适当的屏障C隔开，象是各区的边界，从而能在各区内形成指定的可控气氛，所有这些均用溅射镀膜工艺中熟知的常规装置完成。正如上面所解释的，以前认为当在溅射镀膜操作中用银作靶子时，尽可能地保持该区内(即区3)基本上不含氮很重要。因此，在制备先有技术图2体系的已知方法中，规定要使用100％的氩气氛。过去还认为Si应该在100％的N2中溅镀，因此规定了这一气氛。
于是，使用这种装置和气氛并且通过控制溅射操作的速度和电功率，已知的Airco方法制得了示于图2的这类多层体系。在图2中，有一个玻璃基底“G”。这种玻璃基底最好是约2-6毫米厚的一片玻璃，常常由已知的浮法制得，属于在这种方法中一直使用的典型的钠钙硅酸盐组合物。在区1-2中，形成了主要由Si3N4构成的第一底镀层111。它的公称匣度约为325。区1-2处在基本上100％的N2中。接着使用区3，该区采用基本上100％的氩气氛以便光形成较厚(例如7或更厚)的80/20的镍铬合金层113，接着是较薄的(例如约70)有些不连续的锻层115，它的不连续性由空洞117示明。然后在同一个区3内，在银上镀上另一个较厚的(例如7或更厚)的80/20镍铬层119。随后在区4-5内形成Si3N4的顶镀层121，其厚度稍大于底镀层111(例如约450厚)。上面提到了这种玻璃不够理想的控制阳光的性质，后面在“标准的[std.]Airco”的名称下叙述了它的一个实例。
图3示意说明了可以用图1的装置形成的本发明的两个实施方案。如图所示，在玻璃(2-6毫米厚)基底G上形成了五层。第一层211是Si3N4，在使用基本上100％的N2气氛的的区1-2内形成。任选地，在某些情况下(例如尺寸较小)，可以向例如区2内引入一些氩气以提高Si的溅射。接着，在区3内形成层213(213＇),215，和219(219＇)。
在本发明的一个实施方案中。区3内使用的气氛基本上是100％的氩。在此实施方案中，靶p1(31)最好是80/20镍铬合金，但是也可以根据需要是镍或其它镍基合金。为了获得改进的控制目光的特性并从而克服图2产品所带有的问题，使基本上是纯金属层的层213保持厚度小于约7。这是通过将靶p1(31)上的功率降低到比制造图2产品时使用功率低20％或更多来完成的。然后，作为对图2产物的进一步改进，使靶p2(16)产生的银层215比层115厚(例如厚度为约90-105)，从而使层215基本上连续。这是常规地通过将靶p2的功率增到比制造层115时多20％-33％或者更多来完成的。
接着，按照与层213形成的相同方式，形成另一个基本上是纯金属的80/20镍铬合金(或其它的镍基金属)层，其厚度也相同。随后在区4和5中形成Si3N4顶镀层221，其方式与形成底镀层211的相似。层221常常比层211稍厚。(例如，约540，层211则约400)。虽然本发明的Si3N4底镀层和顶镀层的匣度(例如211和221，或下面提到的311和321)时常与Airco产品中的(例如111和121)相同，但是在本发明的优选实施方案中，与Airco产品相比，它们都加厚了。这是通过将区1-2和4-5的溅射镀膜机的功率增加约20％来实现的，以便达到这些较大的厚度。所得的多层体系的耐久性与图2的多层体系产品近似相同，抗擦伤性稍差，但是辐射率、透射率和薄膜电阻性质比图2产品要优越得多(即，透射率接近80％，辐射率和Rs值则低得多)。
在图3示例说明的另一个特别优选的实施方案中，用采图1的装置和一种独特的方法，达到了甚至更好的控制日光的性质。在这种独特的方法中，遵循对第一实施方案所述的相同的基本步骤，不同之处在于，与先前保持的看法完全相反，在区3内N2气和氩气一起使用，而且靶p1(31)和p3(33)中的一个、最好是两个均用镍-铬合金，从而使铬金属以氯化物的形式沉积在Ni∶Cr层中[即，层213＇和/或219＇中的一层或两层]。在这方面，氩与氮之比可以根据需要变化，但是一般来说，已发现0％-75％体积的Ar对100％-25％的N2，最好是50％-50％Ar对N2，使特性(例如透射率和Rs)提高得比上述本发明第一实施方案还要优越。在此实施方案的优选形式中，各层厚度保持与第一实施方案相同。典型的功率水平在下面报道。
图4中示例说明的多层体系，可以象上述一样通过形成镍基层作为基本上纯金属层来制得，或是使用含N2的氩环境和镍-铬合金作为一个或多个靶，通过在一个或多个(最好是所有的)Ni∶Cr层中产生铬的氯化物来实现改进的结果。另外，在这一实施方案中，图3的单个银层215被夹于其中的镍基层分成两个银层。因此，图4的实施方案可以通过在区3中使用适当数目的靶(未画出)，在区1-2中形成Si3N4底镀层311、在区4-5中形成Si3N4顶镀层321来制得。最好是层311和321的厚度分别与层211和221的相同。
图4与图3的主要区别在于，在区3中先形成厚度小于约7的镍基(即，较好是80/20镍铬合金)金属层313或其氮化物替代物313＇。然后形成约50厚的第一银层315A，接着形成厚度小于约7的另一外镍基金属层314或它的氮化物替代层314＇。随后形成厚度约50的第二银层315B，接着是厚度小于约7的另一个镍基金属层319或其氮化物替代层319＇。在这一方面，应该指出总的银层厚度最好是在约90-105之间。此体系最后用上述的Si3N4顶镀层321完成加工。
正如所预料的，当图4实施方案中的银层315A、B都只有约50厚时，将会产生由空洞317表示的不连续性，就象在图2实施方案中的空洞117一样。虽然这种不连续性在图2中是一种重大的损害，但在图4实施方案的实施中则不然。
图4的七层体系比先前图3的两个实施方案更耐久，虽然它的透射率比这些实施方案低(即，只略高于最低的76％的水平)，但是它的辐射率和Rs值比图3实施方案中的那些好。这一现象的确切原因尚不知道，但是据信将银分成两层并配合使用Ni基(即Ni∶Cr)中间层与此有重大关系。在这一方面，中间的Ni基层被认为是重要的功能屡，它对于达到较强的耐久性有很大的帮助，特别是如果它是Ni∶Cr合金(即80/20镍铬合金)的形式、其中铬又已转化成铬的氮化物时更是如此。
现在根据一些实施例对本发明说明如下：
                      实施例
使用图1的装置制得一个典型的图2示例的标准(“STD”)Airco体系和两个图3示例的实施方案。本发明的第一个实施方案称为类型“A”，第二个(即，氮化物在层213＇中和层219＇中形成)称为类型“B”。对于t1-12和t18-30，所使用的靶是Airco管形掺铝Si靶。靶P1(31)和P3(33)是80％重量的Ni和20％的Cr。靶P2(16)是银(Ag)。所使用的玻璃是Guardian Industries公司制造的常规钠钙硅酸盐浮法玻璃，厚度为3毫米(即，0.123英寸)。采用的线速度为345英寸/分。区1-2和4-5内的压力维持在2.5×10-3乇。在这些区内使用100％N2气氛。在区3内维持压力在2.0×10-3乇。对于“STD”Airco系统和本发明的类型“A”，使用100％氩气氛。对于类型“B”，使用50％/50％的Ar/N2气氛。各个靶的电源如下：
        表1(类型A和B，区1-2和4-5)靶号   伏特   安培 功率(千瓦)1     470    124    58.02     481    115    55.53     431    21     8.94     446    123    55.05     446    124    55.56     449    124    55.57     440    123    54.18     449    130    58.29     429    123    52.710     420    123    51.511     479    30     14.312     450    112    50.419     425    136    57.520     444    135    60.021     453    129    50.622     426    130    55.023     415    104    43.124     441    135    59.525     458    35     16.126     477    138    65.627     455    133    60.528     478    137    58.629     447    86     38.230     429    86     36.8
         表2
   (类型“A”，区3)靶号   犬特   安培   功率(千瓦)31     390    2.6    1.016     447    22.8   10.233     392    2.6    1.0
                表3
          (类型“B”，区3)
靶号    伏特  安培*  功率(千瓦)*
 31     403    5.0    2.0
 16     446    32    14.2
 33     400    5.1    2.0
当产生氮化物时，对于同一膜厚度，功率、安培数和伏特数必须较大。
     表4
(标准，区1-5)靶号     安培      功率(千瓦)1         802         803         804  区1    805         806         80------------7         808         809  区2    8010        8011        8012        80------------------------31        3.8        1.516  区3   18.4       8.133        3.8        1.5------------------------19        13520        10521        12522  区4   12523        10524         25-------------
   表4(续)
(标准，区 1-5)靶号      安培    功率(千瓦)25        12526        12027 区5    5028        11029        11030         80
            表5
         (对照结果)
            玻璃面反射率 膜面反射率多层体系    可见光透射率 (RG)  (RF)类型A    Y(％) 78.75     8.42     4.08施照体C   x    .3097    .2610    .24492°观察   y    .3192    .2722    .2427
      a*  -1.69    -1.64    +1.64
      b*  +1.03    -11.57   -14.68类型B     Y    79.57     7.56     3.75施照体    x    .3089     .2641    .25592°观察   y    .3190     .2709    .2441
      a*   -1.98    -0.40    +3.77
      b*   +0.84    -11.19   -13.45标准      Y     76.45     8.26     5.09施照体C   x    .3078     .2626    .27232°观察   y    .3163     .2801    .2857
      a*   -1.19    -3.25    -1.76
      h*   -0.30    -9.88    -6.95
              表6
          (对照结果)多层体系      En     Eh   Rs(欧姆/平方面积)类型“A”    0.10    0.13    10.0类型“B”    0.10    0.13    9.4标准         0.16    10.20   15.8
作为本发明的另外两个实例和为了显示层的厚度，特别是Ni基层的厚度，对于透射率和红外能反射率能施加的影响，制成了两块类型“B”的玻璃，其作法是在区1和2中和区4及5中使用基本相同的条件，其中于100％N2气氛下形成Si3N4底镀层和顶镀层。区1、2、4和5内的靶是掺Al的Si靶，P1(31)和P3(33)是80/20镍铬合金，P2(16)是银。唯一的不同是在区3中使用如下表所列的不同水平的功率。玻璃是3毫米厚的钠钙硅酸盐型浮法玻璃。
                 表7
         (区3,50/50Ar/N2气氛)
靶(千瓦)                     透射率(施照体C)P1(31) P2(16) P3(33)Rs       Eh    Y％    a*    b*
              玻璃No.11.5     15.0    1.5   8.3      0.11  80.97  -1.88  +1.13
              玻璃No.22.0     14.0    2.0   9.1      0.12  80.02  -1.71  +0.70
可以看出，略微增大两个Ni∶Cr(氮化物)层的厚度和略微减小银层的厚度，红外反射率的透射率值将减小。但是，这两种玻璃对于在建筑用多层窗玻璃中商业使用都合乎要求。
在各个区内使用下面列出的不同水平的功率，形成了类型“A”的玻璃的其它实例。玻璃的厚度为3毫米，是与前面表7中使用的相同的标准浮法玻璃。
            表8                                      透射率
                                                   (施照体C)玻璃编号    靶号      安培    千瓦  Rs   Eh   Y％    a*     b*1        1-12,19-30   85            9.6   0.13  77.11  -2.28  -1.53
        4         35
        31        2.9     1.1
        16                10.2
        33        2.9     1.12        1-3,5-12     85           10.3   0.14  78.02  -2.38  -1.56
      19-30       85
        4         35
       31         2.6    1.0
       16                10.2
       33         2.6    1.03          ＂          ＂    ＂    10.0   0.13  77.84  -2.45  -1.66
       16                10.44          ＂          ＂    ＂     9.8   0.13  79.41  -2.13  -0.30
     19-30        1055      1-3,5-12        90    ＂     9.8   0.13  79.20  -2.10  -0.40
    19-30          90
     4             406        ＂           ＂     ＂     9.8    0.13  79.48  -1.95  +0.17
    19-30         1157      1-3,5-12        95
     19-30        115
       4           40
   31,16,33              ＂     9.7    0.12  79.61  -1.89  +0.058         ＂                 ＂     9.7    0.13  79.78  -1.81  +0.31
     19-30        120
       4          40
   31,16,33              ＂     9.8    0.13  79.95  -1.80  +0.1510   1-3,5-10,12      105           9.8    0.13  79.48  -1.68  +0.66
    19-30         125
       4           95
                   表8(续)
                                                   透射率
                                                  (施照体C)玻璃编号    靶号    安培    千瓦     Rs   Eh   Y％    a*    b*
         11      30
                         ＂11           ＂      ＂      ＂      9.7   0.12  79.66  -1.74  +0.6212      1-2,5-10,12  107             10.1  0.13  79.76  -1.61  +0.68
         3,4     47
         11      32
       19-30    125
       31,33             1.0
        16     10.213*        ＂      ＂       ＂       9.9  0.13  79.60  -1.62  +0.64
*此玻璃特别适合用于商品多层窗玻璃。
在给出了以上公开内容之后，很多其它的特点，变动和改进对于熟练的技术人员将是显而易见的。因此，这些其它的特点、变动和改进被认为是本发明的一部分，本发明的范围由以下权利要求确定。

Claims (21)

1．一种溅射镀膜的玻璃制品，它包括一种玻璃衬底，在该衬底上由玻璃向外有一种多层体系，所述多层体系包含有：
(a)一层Si3N4的底镀层，
(b)一层镍层或镍铬合金层，
(c)一层银层，
(d)一层镍层或镍铬合金层，以及
(e)一层Si3N4顶镀层；
其中，当所述玻璃衬底的厚度为2-6毫米时，所述镀层玻璃具有可见光透射率至少为78％，正常辐射率En小于0.12，半球辐射率Eh小于0.16。
2．根据权利要求1的溅射镀膜玻璃制品，其中所述多层体系基本上由五层构成。
3．根据权利要求1的溅射镀膜玻璃制品，其中，所述多层体系由玻璃向外基本上特别地含有：
(a)一层Si3N4层、
(b)一层镍铬合金层、
(c)一层银层、
(d)一层镍铬合金层、
(e)一层银层、
(f)一层镍铬合金层、以及
(g)一层Si3N4层。
4．根据权利要求3的溅射镀膜玻璃制品，其中，每一个所述银层的厚度均为50，每一个所述镍铬合金层的厚度均小于7。
5．根据权利要求1的溅射镀膜玻璃制品，其中，每一个镍层或镍铬合金层的厚度均小于7，所述制品中只有一个银层，而且所述银层的厚度大于90。
6．根据权利要求5的溅射镀膜玻璃制品，其中，所述银层的厚度为90-105。
7．根据权利要求5的溅射镀膜玻璃制品，其中所述Si3N4底镀层的厚度至少为400，Si3N4顶镀层的厚度至少为540。
8．根据权利要求1的溅射镀膜玻璃制品，其中所述多层体系是耐久的，而且其可见光透射率为78％～80％。
9．根据权利要求8的溅射镀膜玻璃制品，其中所述En为0.10或更小，所述Eh为0.13或更小。
10．根据权利要求9的溅射镀膜玻璃制品，其中所述En是0.09-0.10,Eh为0.12-0.13。
11．根据权利要求8的溅射镀膜玻璃制品，其中所述制品的薄膜电阻为10.5欧姆/平方面积或更小。
12．根据权利要求11的溅射镀膜玻璃制品，其中所述薄膜电阻为9-10欧姆/平方面积。
13．一种溅射镀膜的玻璃制品，它包括一种玻璃衬底，在该衬底上由所述玻璃向外，有一种多层体系，所述多层体系包含有：
(a)一层Si3N4的底镀层，
(b)一层镍铬合金的基底层，它选自镍铬合金和氮化的镍铬合金，
(c)一层银层，
(d)一层镍铬合金基底层，它选自镍铬合金和氮化的镍铬合金，以及
(e)一层Si3N4顶镀层，
其中，至少一个所述镍铬合金基底层是氮化的镍铬合金，而当玻璃衬底厚度为2-6毫米时，镀层玻璃具有可见光透射率至少为78％，其正常辐射率En小于0.12，半球辐射率Eh小于0.16。
14．根据权利要求13的溅射镀膜玻璃制品，其中，所述每一个镍铬合金基底层均是所述氮化的镍铬合金。
15．根据权利要求13的溅射镀膜玻璃制品，其中所述镍铬合金是80重量％的镍和20重量％的铬。
16．根据权利要求15的溅射镀膜玻璃制品，其中，所述透射率是78％至80％，所述En为0.10或更小，所述Eh为0.13或更小。
17．根据权利要求16的溅射镀膜玻璃制品，其中所述镀层玻璃的薄膜电阻为10.5欧姆/平方面积或更小。
18．根据权利要求17的溅射镀膜玻璃制品，其中任何所述的镍毒合金基底层的厚度均小于7A，所述银的总厚度为90-105。
19．根据权利要求18的溅射镀膜玻璃制品，其中只有一个厚度为95的银层。
20．一种溅射镀膜玻璃制品，它包括一种玻璃衬底，在该衬底上由所述玻璃向外，有一种多层体系，所述多层体系包含有：
(a)一层Si3N4的底镀层，
(b)一层镍铬合金的基底层，它选自镍铬合金和氮化的镍铬合金，
(c)一层银层，
(d)一层镍铬合金基底层，它选自镍铬合金和氮化的镍铬合金，
(e)一层银层，
(f)一层镍铬合金的基底层，它选自镍铬合金和氮化的镍铬合金，以及
(g)一层Si3N4的顶镀层，
其中，每个银层的厚度为50，至少一个所述镍铬合金基底层是镍铬合金，当所述玻璃衬底的厚度为2-6mm时，所述镀层玻璃的可见光透射率大于76％，其正常的辐射率En小于0.12，半球辐射率Eh小于0.16。
21．根据权利要求20的溅射镀膜玻璃制品，其中，每一个所述镍铬合金基底层均是氮化的镍铬合金，其厚度小于7，每一个被结合的所述银层的总厚度为90-105，所述镀层玻璃的薄膜电阻为10.5欧姆/每平方面积或更小，所述镍铬合金是80重量％的镍和20重量％的铬，所述透射率是78％-80％，所述En是0.10或更小，所述Eh是0.13或更小。
CN93105250A 1992-04-30 1993-04-30 溅射镀膜的玻璃制品 Expired - Fee Related CN1044358C (zh)

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