CN1074424A - 改进了的可热处理溅射镀膜玻璃层系 - Google Patents
改进了的可热处理溅射镀膜玻璃层系 Download PDFInfo
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Abstract
一种可热处理的溅射镀膜玻璃层系。该层系包
括由镍或一种高镍合金构成的金属层,该金属层上面
镀一层由金属硅或镍的一种氧化物或高镍合金的一
种氧化物构成的隔离层,该隔离层上面镀一层按理论
配比的SnO2这样的金属氧化物的保护层。在热处
理之前,将所说的层系镀到玻璃基板上。
Description
本发明涉及具有特殊镀膜的玻璃,所述镀膜而后可在足够高的温度下进行热处理,以便对其进行弯曲、热强化和/或调质。本发明尤其适用于建筑和汽车工业中的玻璃制造。
在建筑和汽车设计中,金属和金属氧化物镀膜玻璃已被公知。正如在专利文献和其它文献中广泛报道的那样,借助于对镀膜层系的控制,通常通过选择金属和/或金属氧化物和/或层的厚度,一般就能使这种玻璃获得相当满意的反射度、透明性、辐射率和使用寿命及所须要的颜色。例如,在这方面可参见仅列出的几篇美国专利3,935,351;4,413,877;4,462,883;3,826,728;3,681,042;3,798,146和4,594,137。
溅镀这种镀膜的技术已有所报导。这些技术都是可信赖的。其中最有效的因此而被推荐的一种技术是“磁性增强的溅射镀膜”的已有技术。美国专利4,166,018报导了这种技术,这是一有关该技术主题的一种公认的基本技术。(还可参见Munz等人的“现代建筑玻璃镀膜的性能及溅镀规范”SPIE第325卷,光学薄膜1982年65-73页)。
尽管溅射镀膜对许多已知层系是有效的,但采用溅射镀膜仍会导致机械寿命的等级低于由另一种称之为“热分解”技术的方法所获得的机械寿命的等级。而另一方面,溅射镀膜对红外线的反射性又常常优于典型的热分解镀膜。溅射镀膜玻璃通常还被认为具有比热分解形成的镀膜优良的光学和热学性能,如改善了镀膜的均匀性,良好的发射性和较好的阳光特性。显然,如果在提高溅射技术优点的同时为该技术设计出一种特殊的镀膜层系,该层系的机械寿命等级能接近或等于热分解技术的等级,那么将会使现有技术向前跨出明显的一步。在本发明的优选的实施例中,下述的关于此技术主题的发明就会满足该技术领域的多方面的须要。
近几年来,已对普通镀膜玻璃进行了大量尝试,以便获得一种镀膜玻璃产品。这种玻璃可在热处理之前镀膜,然后,在不使其性能变坏的条件下进行热处理。这样作的原因之一是,例如,在已经弯曲的玻璃上得到均匀的镀层是非常困难的。众所周知,如果在平的玻璃表面上进行镀膜,然后弯曲,与先使玻璃管弯曲再进行镀膜的情况相比,使用简单的多的技术就可获得均匀的镀层。
最近已开发出一些用于制造可热处理的玻璃制品的技术。制造这种玻璃制品的方法是,在镀膜后,通过调质、弯曲或一种称之为“热强化”的技术,对其进行热处理。一般说来,许多这些已有技术所具有的缺点是,不是真正在实现经济地弯曲、调质和/或热强化所须要的相当升高的温度(即1150°F-1450°F)下进行热处理的。简言之,这种技术的缺点是,为了在对镀膜玻璃或玻璃基层不产生不利影响的条件下对其进行热处理,要求将热处理温度保持在大约1100°F或更低。
然而在这方面,本发明的两位发明人已在先发明并为销售而提供了一些具有已有技术镀膜层系的玻璃,将这种玻璃在上述的相当高的温度下进行热处理,实现调质,弯曲或热强化。一般地说,这些已有技术的镀膜组成的独特之处是在层系中采用了一金属层。该金属层的一种优选的形式是一种高镍含量的合金,该合金被称为Haynes 214,其成份基本上为:75.45% Ni,4.00% Fe,16.00% Cr,0.04% C,4.50% Al,及0.01% Y(按重量百分数计)。利用高镍合金如Haynes214或者单独用理想配比的氧化锡(SnO2)或者还用其它层(如同样理想配比的氧化锡作底层和/或在SnO2顶层和高镍合金之间的中间层Al)复盖高镍合金,发现在升高的约1150°F-1450°F温度下经约2-30分钟,可获得玻璃产品的热处理性,基本上不降低其颜色、寿命、耐化学腐蚀性、发射性、反射率或透明度。因此,这些组成相对于在下列专利4,790,922;4,816,034;4,826,525;4,715,879和4,857,094中公开的已有的可热处理的层系具有明显的改进。
除在上述专利中公开的上述内容以外,还有Leybold“光谱”挡风玻璃层系TCC-2000也是已知的。在这个层系中,为获得一种溅射镀膜玻璃,采用四或五层金属或金属氧化物,将有这种层系的玻璃在1100°F以下的温度下快速稍微进行热处理后,可作为一种予镀膜玻璃,用于制造弯曲或不弯曲的挡风玻璃。从玻璃基板向外的镀膜通常包括第一层氧化锡,第二层镍/铬合金(一般约为80/20),第三层银,第四层镍/铬合金,和第五层氧化锡。另外,热处理温度和时间上限太低,则所得到的镀膜大软,抗化学腐蚀性很不好,这种镀膜只能用在叠层挡风玻璃的内表面上。
上述的美国专利4,715,879特别指出,除非金属氧化物(例如氧化锡)保护层中的氧化物是缺氧的(即不理想的配比),否则其中的层系就不能实现。当然,这就要求在制造过程中进行精确平衡。在这方面,美国专利4,826,525也公开了可热处理性,然而,这篇专利专门指出,必须采用一层铝以获得可热处理性。
在本发明的实践中,用作高镍含量的合金(即含镍大于约50(重)%的合金)的最优选的合金是由Haynes国际公司生产的称为第214 Haynes合金的一种合金。这是一种以其优秀的耐氧化性、耐碳化性和耐氯化性著称的镍基高温合金。它的标准的化学组分如上所述。尽管这种特别独特的合金及镍和/或其镍含量大于50(重)%的其它合金在本发明的实践中被认为是有用的,但仅用这些合金不能实现由有关这个技术主题的本发明所作的改进。这些改进是由独特的层系实系的,而不是由在其上的和其本身的一特殊层来实现的。
制造建筑或汽车用玻璃,通常采用三种不同的热处理类型,即弯曲、调质和称为“热强化”或“硬化”的简易调质形式。当对普通的1/4”透明浮法玻璃进行弯曲而不调质时,例如,须要在1150°F或更高的温度下持续10-30分钟的时间。在对这种玻璃进行热强化或调质时,进行或不进行弯曲,通常采用高达约1450°F(例如1150°F-1450°F)的温度,持续时间2-5分钟。正如已知的那样,许多已知的或已报导的已有技术都存在着明显的缺点,为了使镀膜玻璃、特别是有效的溅射镀膜玻璃可进行热处理,都对其上限温度作了限定。因此,这里所用的术语“可热处理的”是指镀膜玻璃能够经受一种或多种上面的三种处理,是指在本发明的优选形式中,在1150°F-1450°F的温度下在必须的时间内能够热处理。
在建筑或汽车设计(例如汽车暗窗)中所用的镀膜玻通常具有八种决定其效能和/或销路的特性:商业可行性,寿命(机械耐磨性),耐化学腐蚀性,长期稳定性,发射性,透明性,反射性和颜色。在包括本发明的两个人开发的已有层系中,如上所述,必须注意对一些特性兼顾考虑,以便使其余特性达到令人满意的必须程度。例如,在本发明人的已有层系的情况中,当获得高温可热处理性时,机械寿命便不是最佳数值。因此,由于这个和其它的理由,显然,在这种技术中,对可热处理的在建筑和/或汽车设计中所用的镀膜玻璃存在一种要求,即不要明显放弃上述八个特性中的任何一个,并最好在上限温度和时间内进行热处理(即弯曲,调质和/或热强化)。
对用溅射镀层技术形成的镀膜,要求其同样具有热分解形成的镀层的机械寿命。
本发明的目的是实现上述要求和其它要求,这些其它要求在本领域的普通技术人员看了下述的详细描述后就是明白。
一般地说,本发明通过提供一种可热处理的溅射镀膜玻璃产品来实现这个技术领域中的要求,该溅射镀膜玻璃产品包括一玻璃基板,基板上有镀膜层系,该层系包括下列三层:
(a)一层基本上未氧化的金属层,该层由镍或按重量百分比计镍含量大于约50%的镍合金形成;
(b)一层金属氧化物保护层,其中金属氧化物中的金属与层(a)中的金属不同;和
(c)位于层(a)和层(b)中间的硅或金属氧化物或金属氮化物的隔离层,其中金属氧化物或金属氮化物中的金属是镍或按重量百分比计镍含量大于约50%的镍合金,且层(c)紧密地将层(a)粘附在层(b)上。
在本发明的某优选的形式中,上述的可热处理的玻璃产品包括一玻璃基板,在玻璃基板上有镀膜,该镀膜包括下列五层:
(a)第一层是由从锡,锌,钛和它们的合金选择出的一种金属的氧化物构成;
(b)第二层是由从镍和按重量百分比计镍含量至少约为50%的一种镍合金中选择出的一种金属的氧化物或氮化物构成;
(c)第三层是由从镍和按重量百分比计镍含量至少约为50%的一种镍合金中选择出的一种金属构成;
(d)第四层是由从镍和按重量百分比计镍含量至少约为50%的一种镍合金中选择出的一种金属的氧化物或氮化物构成;
(e)第五层是由从锡,钛和它们的合金中选择出的一种金属的氧化物构成。
在本发明的特别优选的形式中所形成的所有氧化物均为理想配比的。例如,在本发明的某些优选的形式中,上面的第一和第五层实质上由理想配比的锡的氧化物(SnO2)组成,而第二和第四层是和在第三层中使用的金属相同的金属的理想配比的氧化物。
本发明最优选的形式是,用上述的第214号Haynes合金作为第二,三和四层所涉及的金属。当使用这种特殊的合金并采用上述层系时,发现本发明在汽车玻璃领域,特别是在所谓的“暗窗”玻璃领域有独特的用途。
本发明还涉及制造一种可热处理的镀膜玻璃产品的方法,包括从玻璃向外按一定的顺序镀在玻璃基板上溅射镀膜,该镀膜包括下列五层:
(a)任选的第一层是由从锡,锌,钛和它们的合金中选择出的一种金属的氧化物构成;
(b)任选的第二层是由从镍和按重量百分比计镍含量至少约为50%的一种镍合金中选择出的一种金属的氧化物或氮化物构成;
(c)第三层是由从镍和按重量百分比计镍含量至少约为50%的一种镍合金中选择出的一种金属构成;
(d)第四层是由金属硅或由从镍和按重量百分比计镍含量至少约为50%的一种不含硅的镍合金中选择出的一种金属的氧化物或氮化物构成;
(e)第五层是由从锡,锌,钛和它们的合金中选择出的一种金属的氧化物构成。
在本发明的方法的某些优选的形式中,所说诸氧化物层的溅射都要在富氧气氛中进行,从而形成基本上是理论配比的氧化物。各层的优选形式如上面在描述本发明所涉及的可热处理的玻璃产品时所介绍。
用于制造有镀层的热处理了的玻璃产品的方法也包括在本发明的范围内,包括:
(a)形成镍或按重量百分比计镍含量大于约50%的一种镍合金的基本上未氧化的金属层;
(b)在层(a)上独立地形成一层金属硅或一层金属氧化物,其中,所说氧化物中的金属是镍或按重量百分比计镍含量大于约50%的一种镍合金;
(c)在层(b)上独立地形成本质上是理论配比的金属氧化物保护层;和
(d)然后利用在术语“热处理”的定义范围内的一种上述热处理方法对所说的产品进行热处理。
如上所述,所采用的优选的层系是如上所述的层系。在本发明的特别优选的实施例中,这个热处理方法包括,在约1150°F-1450°F的温度范围下,持续足以使所要求的热处理完成所须的时间,来进行这个热处理。当然,这些特别优选的形式还包括采用如上所述的溅射镀膜方法所形成的镀层。本发明还涉及可能应用的各种玻璃,这些玻璃的优选形式是无色或有色的(例如绿色的)浮法玻璃。
本发明还涉及用本发明的上述方法制造的热处理过的玻璃产品。这些产品可以是各种形状和形式的,但在某些优选的实施例中,指的是热处理过的(调过质的,热强化过的和/或弯曲了的)具有那种商业玻璃所要求的特性的汽车暗窗玻璃。
现在参照在下面附图中所表示的本发明的某些实施例对本发明进行描述。
图1是本发明所期望的一种典型镀膜层系的部分剖面图,在优选的实施例中,将该层系镀到汽车暗窗玻璃的基板上。
图2是用于实现本发明的Airco-Temescal三区段建筑溅射镀膜机的示意图。
图3是用于实现本发明的Airco-Temescal五区段建筑溅射镀膜机的示意图。
参见图1,在侧视剖面图中表示出按照本发明的镀膜玻璃制品的一个具型的实例。其中表示出了玻璃基板G和五层层系A-E。下面将对该层系和它的不同的组成予以描述。但首先应明确玻璃基板G可具有多种形状并可是多种类型。然而,在本发明的实践中,基板G最好是典型的浮法玻璃,透明的或有颜色的。当玻璃基板G作为汽车暗窗玻璃(如图1的部分剖面图所示)时,在本发明的实践中,发现绿色是特别优选的。
在本发明的某些实施例中,镀层A和B是优选的。在本发明的实践中,希望镀层C是金属层。该金属层实质上由镍或不含硅的高镍合金构成(即按金量百分比计镍含量大于约50%、而最好大于约70%的不含硅的镍合金)。
本发明所涉及的不仅是纯镍,另外还有如因康镍合金,镍铬合金和其它熟知的高镍含量合金这样的镍合金。然而,用于本发明的特别优选的是所谓的第214号Haynes,这是一种不含硅的高镍合金。这种合金具有上述的标准组份。
层D是实施本发明的特别重要的一层,在本发明中该层不仅作为层C和层E之间的紧密的粘结层,而且能可靠地明显增加本发明的优选实施例的可热处理特性。在这方面、层D是通过溅射镀膜形成的单独的层,该层本质上是由元素硅(Si)或从镍(Ni)或按重量百分比计镍含量大于约50%的一种镍合金(最好不含硅)中选择出的一种金属的一种氧化物(最好是理想配比的)组成的。在本发明的特别优选的实施例中,层D是单独形成的氧化物层,它的金属与形成层C时采用的金属相同。
层E是一层保护层,该层是从由锌、钛、锡和它们的合金组成的组中选择出的一种金属的一种金属氧化物(最好是理想配比的)。然而,在本发明的最佳实施例中,这个保护层E本质上是由理想配比的氧化锡(SnO2)组成。
上面的三层构成了基于本发明实践的基本层。然而,还可增加某些任选层。在本发明的优选的实施例中,已发现这些任选层对本发明所涉及的某些产品来说明显增加其改进的特性。在这方面,层A又可以是将层B粘结到玻璃基板上的另一保护层。因此层A应具有不仅是使层系不受来自玻璃基板G的不良影响的特性,而且还要作为基板G和层B之间的紧密的粘接剂。在本发明的最佳实施例中,层A可以是从与层E的相同组的氧化物中选择出来,在特别优选的实施例中,层A的金属氧化物与层E采用的金属氧化物相同,且在这方面,采用的是最优选的理想配比的氧化锡(SnO2)。
任选的层B除将层C紧密地粘结到层A上以外,还起着和层D相同的作用。层B可以是从与形成层D时采用的金属氧化物相同的金属氧化物中选择的,在这方面,在它的优选的实施例中,指的是与层C中采用的金属相同的金属的一种氧化物。当然,在最优选的形式中,层B,C和D的金属是Hayns 214,而层A和E的金属是锡。
在本发明中采用的用来镀膜的技术可以是任一种已知镀膜技术,但在特别优选的形式中,该技术是上述的溅射镀膜技术,在实现本发明的过程中,溅射镀膜技术中可用任何普通的溅射镀膜机实施,如用已知构造的普通Airco-Temescal多区段建筑溅射镀膜机。如图2所示,这种镀膜机可具有其普通的形式,其中,在三个区段的每个区段中采用三个对电极,因此有对电极1-9。图中所示的平玻璃板(例如以平板的形状,但要被弯曲和/或被调质成为汽车暗窗玻璃)作为玻璃基板g在皮带输送机11上(只是示意地表示出辊形)被输送通过Airco溅射镀膜机,它的区段以已知的形式被壁F隔开,壁F的下端有一个可调的通道T。按常规设置予冲洗装置13和最终冲洗装置15。
由于壁F中有通道T,通过对压力的适当的调节或通过喷嘴O2有选择地增加氧气在内界面上形成氧化物镀层,而在中间区段2内形成基本上没氧化的金属层。因而,例如参照图1中所镀的镀膜作为基板G上的镀膜,当基板G向前通过这三区段的装置时,全部三个对电极1-3可以是相可的保护金属(例如锡)。在这种情况下,区段1内的压力可以调节到约2-3x10-3乇,用80%的O2和20%的氩气作环境气体。作为区段2的对电极可具有层B,C和D所须要的不同的成份,而区段3将具有层E所须要的金属。使区段2内的压力比区段1内的压力低,用100%的氩气作为环境气体(和/或有选择地利用氧化喷嘴O2),然后使区段3内的压力为1.0x10-3-3x10-3乇,就可以按下面的方式形成图1所示的五层。
当玻璃G向前通过处于上述压力下的区段1时,如果这个任选的层是须要的,那么理论配比的氧化锡就作为层A镀到玻璃上。使区段1内的压力高于区段2内的压力,氧气便流到区段2和/或打开第一个喷嘴O2,这样,如果用对电极4来形成任选的属B,从此镀层将被氧化(优选的是按理论配比)。在这方面,对电极4可由因康镍合金、镍铬合金、Haynes 214或其它高镍合金构成。
使对电极5下面的区域缺氧,这样,在单独地形成的层B的上面形成一层基本上是纯的金属层C。因此,对电极5可与对电极4相同,或处于所希望的同一类中。如果希望D层是硅,则对电极6由硅制成,且可控制区段3内的压力,使它低于区段2内的压力(例如1X10-3乇),并将第二个喷嘴O2关闭,这样,就形成了基本是未氧化的硅来作为层D。另一方面,如果要求形成与层B相同的氧化物层D,那么要使区段3内的压力高于区段2内的压力(例如1x10-3乇)和/或将第二个喷嘴O2打开,这样,就形成了一种氧化物(最好是按理论配比)层D。此处,当不希望是硅时,对电极6通常是与对电极4相同的材料或同类材料(且优选的是与对电极5相同的材料)。
然后当玻璃G通过区段3时,对电极7,8和9可提供保护性金属氧化物镀层(例如和层A相同的按理论配比的SnO2)。这样便完成了这种可热处理的镀膜层系。从区段3的端部送出的是牢固粘结的优良的镀膜层系。该层系具有如上面所列举的包括机械寿命在内的突出水平八个特性。在这方面还要指出的是,就本发明的情况而言,无论使用透明浮法玻璃还是绿色浮法玻璃,无论采用什么形式,不管是在热处理之前还是在热处理期间,层C都不改变玻璃基板的折射指数。
从图2可以明显看出,还可采用其它对电极的变换和组合。例如,宁可不依靠区段间的压差和/或使用喷嘴O2,而利用对电极3和/或7来完成帮助形成保护层之外的目的。那么,在一实施例中,对电极1-2和8-9可以是Sn,而对电极3-7是Haynes 214。各区段内的压力基本上相等(和/或既不采用对电极4,也不采用对电极6),可形成本发明所涉及的一个五层膜的层系,因为在形成SnO2的相同的层中形成了Haynes 214氧化物。当然,在另一个实施例中,对电极6应是Si而对电极7应是不起作用的,因此形成了本发明的另一种镀膜层系。一了解已公开的内容,各种其它组合对普通技术人员来说是显而显见的。
图3表示用于形成上述镀膜层系的可供选择的工序。在这于实施例中,采用普通的五区段Airco-Temescal溅射镀膜机。使用十五个对电极中的九个对电极1-9(或使用全部十五个对电极)。另外,在这个实施例中,对电极1-3和7-9最好是金属的,用来作为保护氧化物(例如最好是按理论论配比的氧化锡SnO2),当然,在此亦可采用上面所推荐的各种变换和组合,因为有十五个对电极。
这个实施例和图2所示的实施例之间的区别在于,本实施例给每个单独的层提供一个单独的区段,不同的压力和/或不使用专门的氧化喷嘴O2。在这方面,通常所须要的就是以公知的形式控制一个适当的气压以便在任一个区段中得到的所须要的结果。例如,在全部五个区段中可采用一个大约为2x10-3乇的公称压力,然后,既可采用100%的氩的气氛,又可采用80%的O2和20%的氩的气氛,从而既可形成基本上是金属的层(100%的氩),又可形成按理论配比的氧化物镀膜(80%的O2,20%Ar)。当然,在此应该明确为了得到特别的结果,象对图2的实施例所描述的那样,如果须要,可有选择地采用不同的压力和/或喷嘴O2(未画出)。还应明确,就这两个实施例而言,为获得一种特别的结果,如厚度,速度等等,可改变所采用的对电极的数目。所有这些对于熟悉溅射镀膜技术的普通技术人员来说都是熟知的。
按照简单的试验和错误的技术,当改变厚度以便取得所须要的最终结果时,对本发明来说最好使各层的厚度保持在下述常规范围内:
层 厚度(埃)
A 约0-1000(采用时>1)
B 约0-100(采用时>5)
C 约20-250
D 约5-100
E 约20-1000
尽管没有完全理解发明主题的基本原理和它的独特的镀膜层系同时实现了高度的热处理性和机械寿命所借以的作用机理,然而应该相信,下面的条件和用途在正常情况下是适用的:
层的用途:
层E:a)在热处理过程中减少金属层C的氧化性
b)增加叠层的耐磨性
c)增加叠层的耐化学腐蚀性
d)调节叠层的光学特性
层D:a)增强层E和层C间的粘结
b)略微地调节叠层的光学特性
c)增加层系的耐化学腐蚀性
层C:a)反射红外线辐射
b)反射可见光
c)减少太阳能传导
d)减少可见光传导
e)在热处理过程中耐高温氧化
层B:a)增强层C和层A间的粘结
b)略微地调节叠层的光学特性
c)增加层系的耐化学腐蚀性
层A:a)减少可见光在玻璃侧的反射
b)在高温下减少层C和玻璃基板间的相互作用
c)在玻璃表面上减少层C对光蚀的敏感性(由于水份对玻璃的侵蚀)
d)增加层系的耐化学腐蚀性
c)调节颜色
例1
(图2,对电极1-3,7-9是Sn;对电极4-6是Haynes214合金。玻璃:绿色浮法玻璃)
典型的工艺条件:
层E: (优选的)
工作气体: 氩和氧 (80%的O2,20%的Ar)
气体压力: 0.5-5.0×10-3乇 (1.0×10-3乇)
对电极电压: 200-800伏 (393伏)
对电极电流: 可变 (7.4安)
对电极功率: 可变 (2.9KW)
层D:
工作气体: 氩和氧 (50%的O2,50%的Ar)
气体压力: 0.5-5.0×10-3乇 (8.9×10-4乇)
对电极电压: 200-800伏 (347伏)
对电极电流: 可变 (7.4安)
对电极功率: 可变 (2.6KW)
层C:
工作气体: 氩和氧 (14%的O2,86%的Ar)
气体压力: 0.5-5.0×10-3乇 (7.7×10-4乇)
对电极电压: 200-800伏 (407伏)
对电极电流: 可变 (7.9安)
对电极功率: 可变 (3.2KW)
层B:(与层D相同)
层A:(与层E相同)
典型的光学和电学特性:
(关于5/32"(4.0mm)绿色浮法玻璃的特性)[在调质炉中焙烧以后]
可见光透明度: 20-23%Ill。C,2° 观察器
可见光反射率(玻璃侧): 11-12%Ill。C,2° 观察器
可见光反射率(镀膜侧): 31-33%Ill。C,2° 观察器
可见光颜色(玻璃侧): 灰色a=0.5,b=0.8
可见光颜色(镀膜侧): 金色a=1.0,b=24.0
辐射率: 0.37-0.38
层阻: 35-37Ω每平方
阳光透射率: 13-14%
阳光 反射率: 10%
例2
(图2,对电极1-3,8-9是Sn;对电极4-7是Haynes214合金,但对电极7是不起作用的。玻璃是5/32"有色浮法玻璃。)
典型的工艺条件:
区段 对电极 KW 伏 安 材料 压力 气氛(O2%Ar%)
1 1 20 421 45 Sn 2x10-3(乇) 80/20
1 2 19 428 45 Sn 2x10-3(乇) 80/20
1 3 19 427 45 Sn 2x10-3(乇) 80/20
2 4 2 348 10 214 2x10-3(乇) 100%Ar背景气体O2
2 5 17 515 31.5 214 2x10-3(乇) 100%Ar
2 6 5 371 10 214 2x10-3(乇) 100%Ar背景气体O2
3 7 - - - 214 2x10-3(乇) 80/20
3 8 14 390 21 Sn 2x10-3(乇) 80/20
3 9 12 399 34 Sn 2x10-3(乇) 80/20
在这个实施例中,在第四和第五对电极处采用喷嘴O2(例如约为149标准立方厘米),以便确保Haynes 214合金在这些地方被氧化。所用的有色玻璃是普通的绿色浮法玻璃,这种玻璃进行调质,硬化和/或弯曲的转变温度约为1140°F-1160°F。冲洗器的速度设定为70.0%。在这三个区段内的放出的气/背景气体分别为1099/275,480/149和893/222标准立方厘米。在区段2内只打开用于对电极4和6的背景气体管(即喷嘴O2)。为了确保对极5的Haynes 214基本上不被氧化,保持电压大于505伏。所得到的镀膜有五层,从玻璃向外其基本组成是:SnO2/214氧化物/214金属/214氧化物/SnO2。可以确认,所有的氧化物基本上都是按理论配比的氧化物。
然后把用典型的板画方法涂镀的呈未弯曲的汽车暗窗玻璃的形式的这种玻璃件放到温度约为1240°F-1330°F的炉子中,对其进行通常的调质和弯曲处理,持续足够的时间,得到成品。该成品就是一种优良的汽车暗窗玻璃,从玻璃侧看呈中灰色,从镀膜侧看呈金色,并且有很好的寿命特性。
例3
除使对电极6不起作用而使对电极7起作用外,利用例2中所述的工艺,可形成类似于例2的一种汽车暗窗玻璃。这种暗窗玻璃具有优良的性能,经久耐用。
从上面所述可以看出,采用本发明的独特的镀膜层系和方法可获得优良的机械寿命,光学和可热处理特性。然而,对普通技术人员来说,一了解上面公开的内容,各种其它的改变,特征或改进就成显而易见。因此这些其它的特征,改变和改进是本发明的一部分,本发明的保护范围由下面的权利要求确定。
Claims (34)
1、一种可热处理的玻璃产品,包括一玻璃基板,在基板上有镀膜,该镀膜包括下列四层:
a)第一层是由从镍及按重量百分比计镍含量至少约为50%的一种镍合金组成的组中选择出的一种金属的一种氧化物或氮化物构成;
b)第二层是由从镍和按重量百分比计镍含量至少约为50%的一种镍合金组成的组中选择出的一种金属构成;
c)第三层是由从镍和按重量百分比计镍含量至少约为50%的一种镍合金组成的组中选择出的一种金属的一种氧化物或氮化物构成;
d)第四层是由从锡,锌,钛和它们的合金组成的组中选择出的一种金属的一种氧化物构成。
2、一种可热处理的玻璃产品,包括一玻璃基板,在基板上有镀膜,该镀膜包括下列五层:
a)第一层是由从锡,锌,钛和它们的合金组成的组中选择出的一种金属的一种氧化物构成;
b)第二层是由从镍和按重量百分比计镍含量至少约为50%的一种镍合金组成的组中选择出的一种金属的一种氧化物或氮化物构成;
c)第三层是由从镍和按重量的分比计镍含量至少约为50%的一种镍合金组合金组成的组中选择出的一种金属;
d)第四层是由从镍和按重量的分比计镍含量至少约为50%的一种镍合金组成的组中选择出的一种金属的一种氧化物或氮化物构成;
e)第五层是由从锡,钛和它们的合金组成的组中选择出的一种金属的一种氧化物构成。
3、一种按权利要求2的可热处理的玻璃产品,其特征在于,所说的第一和第五层基本上由氧化锡构成。
4、一种按权利要求2的可热处理的玻璃产品,其特征在于,所说的第二、三和四层的金属是相同的金属。
5、一种按权利要求4的可热处理的玻璃产品,其特征在于,第一和五层基本上由按理论配比的氧化锡构成。
6、一种按权利要求5的可热处理的玻璃产品,其特征在于,所说的第二、三、四层的所说金属基本上由按重量百分比计镍含量大于约70%的一种镍合金构成。
7、一种按权利要求2的可热处理的玻璃产品,其特征在于,所说的第一和第五层基本上由按理论配比的氧化锡构成,所说的第三层基本上由包括Ni,Fe,Cr,C,Al和Y的一种合金构成,所说的第二和第四层基本上由第三层的所说合金的一种氧化物构成。
8、一种按权利要求6的可热处理的玻璃产品,其特征在于,所说的第三层是一种基本上由下列成分组成的合金:
成份 (%)重量
Ni 约75.45
Fe 约4.00
Cr 约16.00
C 约0.04
Al 约4.50
Y 约0.01
9、一种按权利要求2的可热处理的玻璃产品,其特征在于,所说的玻璃基板是绿色浮法玻璃。
10、一种按权利要求8的可热处理的玻璃产品,其特征在于,所说的玻璃产品从玻璃一侧看呈中灰色,从镀膜一侧看呈金色,所说的各层的厚度约为:
层 厚度(埃)
1 1-1000
2 5-100
3 20-250
4 5-100
5 20-1000
所说的玻璃产品是一种汽车暗窗玻璃。
11、一种制造一种可热处理的镀膜玻璃产品的方法,包括在所说的玻璃上从玻璃向外按一定顺序溅射镀膜,该镀膜具有下列的各层:
a)第一层是由从镍和按重量百分比计镍含量至少约为50%的一种镍合金组成的组中选择出的一种金属的一种氧化构或一种氮化物构成;
b)第二层是由从镍和按重量百分比计镍含量至少约为50%的一种镍合金组成的组中选择出的一种金属构成;
c)第三层是由从镍和按重量百分比计镍含量至少约为50%的一种镍合金组成的组中选择出的一种金属的一种氧化物或一种氮化物构成;
d)第四层是由从锡,锌,钛和它们的合金组成的组中选择出的一种金属的一种氧化物构成。
12、一种按权利要求11的方法,其特征在于,在所说的玻璃上首先溅镀所说的第一层,第五层是从由锡,锌,钛和它们的合金组成的组中选择出的一种金属的一种氧化物,每个所说的氧化物层的溅射镀膜都要在富氧气氛中进行处理,从而形成基本上是理论配比的氧化物。
13、一种按权利要求12的方法,其特征在于,在进行所说的镀膜以后,在约1150°F-1450°F的温度下,对所说的玻璃产品进行热处理。
14、一种按权利要求13的方法,其特征在于,所说的热处理包括对所说的玻璃进行调质的步骤。
15、一种按权利要求13的方法,其特征在于,所说的热处理包括对所说的玻璃进行弯曲的步骤。
16、一种按权利要求13的方法,其特征在于,所说的热处理包括对所说的玻璃进行热强化的步骤。
17、一种按权利要求12的方法,其特征在于,所说的第五和第四层基本上由氧化锡构成,所说的第二层基本上由按重量百分比计镍含量大于约70%的一种镍合金构成,所说的第一层和第三层基本上是由所说的第二层的合金的一种氧化物构成。
18、一种按权利要求17的方法,其特征在于,所说的第二层基本上由包括Ni,Fe,Cr,C,Al和Y的一种合金构成。
19、一种按权利要求18的方法,其特征在于,所说的第二层是一种基本上由下列成分组成的合金:
成份 (重)%
Ni 约75.45
Fe 约4.00
Cr 约16.00
C 约0.04
Al 约4.50
Y 约0.01
20、一种可热处理的溅射镀膜玻璃产品,包括-玻璃基板,在基板上有一层系,该层系包括下列三层:
a)由镍或按重量百分比计镍含量大于约50%的镍合金形成的基本上没被氧化的金属层;
b)金属氧化物保护层,其中,金属氧化物中的金属与层(a)中的金属不同;
c)在层(a)和层(b)之间的隔离层,基本上由金属硅或一种金属氧化物或氮化物构成,其中,金属氧化物或氮化物中的金属是镍或按重量百分比计镍含量大于约50%的镍合金,其中,层(c)将层(a)紧密地粘结到层(b)上。
21、一种按权利要求20的可热处理的溅射镀膜玻璃产品,其特征在于,所说的层(c)的氧化物中的金属与层(a)中的金属相同。
22、一种按权利要求21的可热处理的溅射镀膜玻璃产品,其特征在于,所说的层(b)基本上由按理论配比的氧化锡(SnO2)构成。
23、一种按权利要求22的可热处理的溅射镀膜玻璃产品,其特征在于,还包括层(d)和(e),其中层c是镍或按重量百分比计镍含量大于约50%的一种镍合金的一种金属氧化物或氮化物,层(e)是与层(b)相同的金属氧化物,层(d)是与层(c)相同的金属氧化物,层(e)将层(c)紧密地粘结到所说的玻璃基板上,层(d)将层(e)紧密地粘结到层(a)上。
24、一种按权利要求23的可热处理的溅射镀膜玻璃产品,其特征在于,所述的产品是汽车暗窗玻璃。
25、一种制造镀膜的可热处理的玻璃产品的方法,包括:
a)形成一基本上没被氧化的金属层,该层基本上由镍或按重量百分比计镍含量大于50%的镍合金构成;
b)在层(a)上单独形成一层,该层是从硅或一种金属氧化物或氮化物中选择出的,其中,所说氧化物中的金属是镍或按重量百分比计镍含量大于约50%的一种镍合金。
c)在层(b)上单独形成一层保护层,该层基本上是按理论配比的金属氧化物,然后,对所说的产品进行热处理。
26、一种按权利要求25的方法,其特征在于,进一步包括,在所说的玻璃产品上先形成一层与层c相同的氧化物层(d),然后在(d)上形成一层与层(b)相同的氧化物层(e),以便层(e)将层(a)紧密地粘结到层(d)上,层(d)将层(e)紧密地粘结到所说的玻璃产品上,所说的层(b)中的金属是镍或按重量百分比计镍含量大于50%的无硅镍合金。
27、一种按权利要求26的方法,其特征在于,在所说的热处理是从调质,弯曲,热强化或它们的组合选择出的,层(c)和(d)基本上由按理论配比的氧化锡(SnO2)构成,层(b)和(e)中的金属与层(a)的金属相同。
28、一种按权利要求27的方法,其特征在于,在所说的玻璃产品是一种弯曲的汽车暗窗玻璃,所说的层(a)的金属是一种基本上由Ni,Fe,Cr,C,Al和Y构成的一种合金。
29、一种按权利要求27的方法,其特征在于,在所说的玻璃是一种绿色浮法玻璃,所说的汽车暗窗玻璃从玻璃一侧看呈中灰色,从镀膜一侧看呈金色,其阳光透射率约为13-14%,阳光反射率约为10%。
30、一种按权利要求29的方法,其特征在于,所说的各层从玻璃向外按下面的顺序排列,各层的大致厚度范围如下:
层 大致厚度(埃)
d 1-1000
e 5-100
a 20-250
b 5-100
c 20-1000
31、一种按权利要求30的方法,其特征在于,所说的层(a)基本上不使玻璃的折射率变坏。
32、一种按权利要求25的方法制造的产品。
33、一种按权利要求27的方法制造的产品。
34、一种按权利要求30的方法制造的产品。
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US07/804,017 US5229194A (en) | 1991-12-09 | 1991-12-09 | Heat treatable sputter-coated glass systems |
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JP (1) | JP2588818B2 (zh) |
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CN (1) | CN1074424A (zh) |
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AU (1) | AU648939B2 (zh) |
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CA (1) | CA2084966C (zh) |
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DE3869270D1 (de) * | 1987-08-08 | 1992-04-23 | Leybold Ag | Verfahren zum herstellen von scheiben mit hohem transmissionsverhalten im sichtbaren spektralbereich und mit hohem reflexionsverhalten fuer waermestrahlung sowie durch das verfahren hergestellte scheiben. |
DE8713181U1 (de) * | 1987-10-01 | 1987-11-26 | Rittershaus & Blecher Gmbh, 5600 Wuppertal | Hochdruck-Filterpresse mit einer Abspritzeinrichtung |
DE3902596A1 (de) * | 1989-01-28 | 1990-08-02 | Flachglas Ag | Verfahren zum herstellen einer vorgespannten oder gebogenen glasscheibe mit rueckseitiger beschichtung, danach hergestellte glasscheibe sowie deren verwendung |
US5217753A (en) * | 1989-02-21 | 1993-06-08 | Libbey-Owens-Ford Co. | Coated glass articles |
JPH02225346A (ja) * | 1989-02-27 | 1990-09-07 | Central Glass Co Ltd | 熱線反射ガラス |
CA2009863C (en) * | 1989-03-09 | 2002-04-30 | Raymond Nalepka | Heat treatable sputter-coated glass |
DE4018399A1 (de) * | 1990-06-08 | 1991-12-19 | Leybold Ag | Verfahren zur beschichtung eines substrats, insbesondere einer glasscheibe, um eine opakwirkung zu erzielen und durch das verfahren beschichtete substrate |
EP0511901B1 (fr) * | 1991-04-30 | 1996-03-06 | Saint-Gobain Vitrage | Substrat en verre revêtu de multicouches minces pour la protection solaire |
-
1991
- 1991-12-09 US US07/804,017 patent/US5229194A/en not_active Expired - Lifetime
-
1992
- 1992-11-25 AU AU29656/92A patent/AU648939B2/en not_active Ceased
- 1992-11-28 TW TW081109544A patent/TW212166B/zh active
- 1992-12-01 HU HU9203790A patent/HU212434B/hu not_active IP Right Cessation
- 1992-12-01 MX MX9206919A patent/MX9206919A/es not_active IP Right Cessation
- 1992-12-02 KR KR1019920023047A patent/KR960015963B1/ko not_active IP Right Cessation
- 1992-12-04 DK DK92120717.1T patent/DK0546470T3/da active
- 1992-12-04 EP EP92120717A patent/EP0546470B1/en not_active Expired - Lifetime
- 1992-12-04 AT AT92120717T patent/ATE140209T1/de not_active IP Right Cessation
- 1992-12-04 ES ES92120717T patent/ES2090468T3/es not_active Expired - Lifetime
- 1992-12-04 DE DE69212126T patent/DE69212126T2/de not_active Expired - Lifetime
- 1992-12-07 JP JP4351347A patent/JP2588818B2/ja not_active Expired - Lifetime
- 1992-12-07 NZ NZ245387A patent/NZ245387A/en unknown
- 1992-12-08 NO NO92924752A patent/NO924752L/no unknown
- 1992-12-08 SK SK3607-92A patent/SK279355B6/sk unknown
- 1992-12-08 CZ CS923607A patent/CZ282482B6/cs not_active IP Right Cessation
- 1992-12-08 ZA ZA929505A patent/ZA929505B/xx unknown
- 1992-12-08 PL PL92296876A patent/PL171372B1/pl unknown
- 1992-12-09 CA CA002084966A patent/CA2084966C/en not_active Expired - Lifetime
- 1992-12-09 BR BR9204960A patent/BR9204960A/pt not_active Application Discontinuation
- 1992-12-09 CN CN92115388A patent/CN1074424A/zh active Pending
-
1993
- 1993-06-24 US US08/080,787 patent/US5298048A/en not_active Expired - Lifetime
-
1996
- 1996-09-13 GR GR960402395T patent/GR3021036T3/el unknown
Cited By (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN100357207C (zh) * | 2000-11-25 | 2007-12-26 | 法国圣戈班玻璃厂 | 具有层叠金属反射薄层的透明基材 |
CN1950534B (zh) * | 2004-05-06 | 2011-12-07 | Ppg工业俄亥俄公司 | Msvd涂覆方法 |
CN105196657A (zh) * | 2014-12-30 | 2015-12-30 | 慧智科技(中国)有限公司 | 玻璃用涂层结构 |
CN105196657B (zh) * | 2014-12-30 | 2017-08-29 | 慧智科技(中国)有限公司 | 玻璃用涂层结构 |
CN106024642B (zh) * | 2015-03-25 | 2019-04-05 | 英飞凌科技股份有限公司 | 用于制造电路载体装置的方法 |
Also Published As
Publication number | Publication date |
---|---|
US5229194A (en) | 1993-07-20 |
NO924752D0 (no) | 1992-12-08 |
US5298048A (en) | 1994-03-29 |
JPH0680441A (ja) | 1994-03-22 |
AU648939B2 (en) | 1994-05-05 |
DE69212126D1 (de) | 1996-08-14 |
SK279355B6 (sk) | 1998-10-07 |
PL296876A1 (en) | 1993-07-12 |
ZA929505B (en) | 1993-06-15 |
HUT66540A (en) | 1994-12-28 |
EP0546470B1 (en) | 1996-07-10 |
NO924752L (no) | 1993-06-10 |
EP0546470A1 (en) | 1993-06-16 |
HU9203790D0 (en) | 1993-04-28 |
KR930012616A (ko) | 1993-07-20 |
JP2588818B2 (ja) | 1997-03-12 |
DK0546470T3 (da) | 1996-08-19 |
BR9204960A (pt) | 1993-06-15 |
DE69212126T2 (de) | 1996-11-28 |
ATE140209T1 (de) | 1996-07-15 |
KR960015963B1 (ko) | 1996-11-25 |
MX9206919A (es) | 1993-06-01 |
CA2084966A1 (en) | 1993-06-10 |
CZ282482B6 (cs) | 1997-07-16 |
CZ360792A3 (en) | 1993-10-13 |
NZ245387A (en) | 1994-04-27 |
TW212166B (en) | 1993-09-01 |
HU212434B (en) | 1996-06-28 |
SK360792A3 (en) | 1994-04-06 |
PL171372B1 (en) | 1997-04-30 |
ES2090468T3 (es) | 1996-10-16 |
AU2965692A (en) | 1993-06-10 |
GR3021036T3 (en) | 1996-12-31 |
CA2084966C (en) | 1998-02-24 |
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