CN1842500A - 涂有介电层的基材及其制造方法和制造装置 - Google Patents
涂有介电层的基材及其制造方法和制造装置 Download PDFInfo
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Abstract
本发明涉及其上面涂有至少一层电介质薄层的诸如玻璃基材的基材(1)。按照本发明,借助于比如磁场辅助和优选在氧和/或氮存在下的反应性的阴极雾化,在曝露在来源于离子源(4)的至少一束离子束(3)的条件下沉积电介质层。本发明的特征在于,所述曝露在离子束下的电介质层被结晶。
Description
本发明涉及借助于真空沉积技术,在透明的基材上,特别是在玻璃基材上沉积的基于电介质的薄层,特别是金属氧化物、氮化物或氮氧化物类型薄层的涂层领域。
本发明涉及被涂布的基材、该基材的制造方法、制造装置及基材涂敷和/或窗玻璃的制造方法,特别是包括至少一层按照本发明基材的双层窗玻璃或夹层窗玻璃的制造方法。
实际上,为了制造所谓“功能性”窗玻璃,一般是在它所包含的至少一块基材上层积一层薄层或一叠薄层,以赋予该窗玻璃以比如抗反射性能的光学性能、在红外区的性能(低发射性)和/或导电性能。比如在银层或掺杂的金属氧化物层的两侧经常使用基于氧化物和/或氮化物电介质的薄层,或者在交替具有低折光指数和高折光指数的一叠薄层中作为干涉层。
一般认为通过阴极雾化所沉积的层,其耐化学品性能和机械性能要比裂解途径沉积的层更差。因此,开发了离子束辅助沉积的实验技术,在该技术中,用比如氧或氩的离子束轰击一个层,这能够增加其紧密的程度以及该层与基材载体的粘接。由于一方面离子束来源于很局限的离子源,而另一方面来自靶蒸发或雾化而产生的颗粒,由于这两者交汇而产生的问题,使此技术长时间来只能应用于尺寸很小的基材。
文献EP601928公开了首先在一个雾化容器中沉积一个层,然后在其沉积了以后,用来源于点离子源的“低能”离子束轰击此介电层,此离子束的能量能够限制在离子束的离子冲击下的雾化,一般为小于500eV,在一百个eV左右。
此处理的目的主要是通过使该层致密化来增加该层的物理和/或化学的耐久性,能够得到该层表面的更小的粗糙度,这就有利于“铺上”沉积在其上面的后面的层。
然而此处理方法具有的缺点是只能在已完全沉积的层上操作。
此处理方法的另一个缺点是只能使如此处理的层致密化,而且此致密化会促使如此处理的层的反射指数增大。因此,如此处理的层不能替代没有处理的层,因为它们的光学性能不同,这就意味着要完全重新定义层的体系,其中包括应有的材料。
另外,此处理没有对在大尺寸基材上的操作进行优化,比如对于制造建筑窗玻璃。
再有,此方法与阴极雾化的方法,特别是由磁场辅助的,优选在氧和/或氮存在下的反应性的阴极雾化方法是完全不相容的,特别是由于处理的压力非常不同:在此发明的时期,离子源在阴极雾化,特别是由磁场辅助的,优选在氧和/或氮存在下的反应性的阴极雾化方法所用压力的1/10~1/100以下操作。
更近一些时候,开发了一种与阴极雾化进行层沉积的方法更好相容的离子源,特别解决了粒子束交汇的问题,改善了一方面是阴极的尺寸和几何形状,另一方面是离子源之间的适应性。此系统被称为“线性离子源”,具体在US 6,214,183或US 6,454,910中有所叙述。
文献WO 02/46491叙述了此类源对于使用氧离子束轰击,通过阴极雾化从银靶制造氧化银功能层的应用。离子束被用来使银材料致密化,并将其转变为含有氧化银的层。由于致密化,明显使得氧化银层能够吸收和/或反射紫外线。
本发明的目的是克服先有技术的缺点,提供一种能够用来涂布玻璃型透明基材的新型薄层材料、新的沉积方法和新型装置。
本发明基于这样一个事实,即能够通过曝露在离子束中,通过控制条件来沉积电介质,特别是氧化物和/或氮化物的薄层,使得最终薄层的材料具有更好的结晶度,远高于在传统条件下,即该层没有受到至少离子束照射的被沉积材料的结晶度。
在此方面,本发明的一个目的特别是按照权利要求1的玻璃基材。按照本发明的该基材通过阴极雾化,特别是通过磁场辅助和优选是在氧和/或氮存在下的反应性雾化被涂布至少一层电介质薄层,该电介质薄层曝露于至少一种来源于离子源的离子束,以曝露于离子束而沉积的电介质层被结晶化。
所谓“结晶化”指的是至少30%的曝露在离子束下的该电介质层的组成材料被结晶化,而且雏晶的尺寸可以通过X射线衍射而检出,即存在有直径大于几个纳米的雏晶。
用来实施本发明的离子束是所谓“高能”离子束,其具有的能量一般在几百至几千个eV的数量级。
有利地控制参数,使得曝露在离子束下通过阴极雾化在基材上沉积的电介质层具有很小的粗糙度。
所谓“很小的粗糙度”指的是曝露在离子束下的电介质层的粗糙度比没有曝露在离子束下的同样电介质层的粗糙度小至少20%,优选至少50%。
因此对于10nm的厚度,曝露在离子束下的电介质层可以具有小于0.1nm的粗糙度。
还可以有利地控制参数,使得该层具有远小于或远大于在没有离子束下沉积的层的指数,但也可以接近在没有离子束下沉积的层的指数。
在本说明的意义上,“接近”指数偏离参考值最多大约5%。
本发明还能够在被沉积的层中建立指数的梯度。
因此在一个实施方案中,所述层具有按照离子源的参数调节的指数梯度。
有利的是,对于至少一部分能够被沉积的电介质材料,无论指数如何改变,在曝露在离子束下通过阴极雾化而沉积在基材上的电介质层的密度能够保持接近或相同。
在本说明的意义上,“接近”的密度值与参考值的偏差最大为大约10%。
本发明特别用来制造化学计量量或非化学计量量的金属氧化物或氧化硅的电介质层或者金属或硅的氮化物或氮氧化物的电介质层。
电介质层特别能够用选自下面的至少一种元素的氧化物制造:硅、锌、钽、钛、锡、铝、锆、铌、铟、铈和钨。在可以设想的混合氧化物中,可特别举出氧化铟锡(oxyde d’indium et d’étain)(ITO)。
可以由掺杂金属,即含有少量元素的金属的阴极得到该层:作为说明,通常使用含有少量其它金属,比如铝或镓的锌阴极。在本说明中,氧化锌理解为可含有少量其它金属的氧化锌。对于提到的其它氧化物也是同样的。
比如,按照本发明沉积的氧化锌层,其结晶度可高于90%,特别高于95%,其RMS粗糙度小于1.5nm,特别小于大约1nm。
按照本发明的此氧化锌层,其折光指数可调节得小于或等于1.9,特别是大约1.35~1.95。其密度可保持在接近5.3g/cm3,特别是大约5.3±0.2g/cm3的值,这与在低压下沉积的ZnO层的密度大约5.3g/cm3是同样的。
将其折光指数调节到小于或接近1.88的氧化锌层可以通过调节阴极雾化的条件(特别是大气中的氧含量)来得到,使其与旨在补偿离子轰击影响的化学计量量的氧化物有很小的偏差。
电介质层还可以是由氮化硅或氮氧化硅制造的。这样的氮化物电介质层可以通过调节阴极雾化的条件(特别是大气中的氮含量)来得到,使其与旨在补偿离子轰击影响的化学计量量的氮化物有很小的偏差。
一般说来,离子束具有改善电介质层机械性能的效果。
通过离子轰击,在电介质层中引入了一定量的轰击物质,其含量取决于源中混合气体的性质,还取决于源/阴极/基材的结构形状。作为说明,在氩离子束轰击下沉积的层,其氩的含量为大约0.2~0.6%(原子),特别是大约0.45%(原子)。
由使用软铁或各种其它金属材料,特别是顺磁材料(在工艺进行的过程中被销蚀)阴极的离子源产生离子束会致使在沉积的层中有痕量铁存在。已经证实,低于3%(原子)或更低的铁含量是可以接受的,因为这不会干扰电介质层的特别是光学性能或电学性能的性能。有利地调节沉积参数(特别是基材的输送速度),会使得铁的含量低于1%(原子)。
由于维持了通常的光学性能,就很容易将如此得到的电介质层放入用来制造所述功能玻璃的已知叠层中,特别是对使用银基金属的功能层。
可以设想通过放入其指数被调节到与标准值不同的电介质层来制造特别的叠层。
因此本发明的目的是一种涂有叠层的基材,其中银层被沉积在曝露在离子束下的所述电介质层的上面。随后至少可将另一层电介质层沉积在此银层的上面。
当下面的电介质层是基于氧化锌和/或氧化锡时,这种结构形状显示出是特别有利的,因为这导致银层在氧化物层上生长时很好地取向,改善其最终性能。在银层下面有氧化锌层存在特别会影响所述银层的质量是众所周知的。在按照本发明沉积的氧化锌层上面形成银层会提供特别明显的改善。
实际上可以观察到,如此形成的银层,其结晶度得到改善,与无定形相相比((111)平面的衍射),晶相增加达15~40%。
在此方面,本发明的另一个目的是改善按照本发明沉积在电介质层上面,特别是在基于氧化锌电介质层上面的银层结晶状况的方法,按照该方法,通过阴极雾化,特别是通过磁场辅助和优选在氧和/或氮存在下的反应性的阴极雾化,将其曝露在至少一种优选来源于线性离子源的离子束下,在基材上沉积所述电介质层。按照此方法,在所述电介质层上沉积至少一种特别基于银的功能层,并使所述功能层结晶。由此可以增大银层雏晶的尺寸大约15~40%,特别是30~40%((111)平面衍射)。
这表现在银电阻的降低(直接与能量发射性能有关),即在同样厚度的银的情况下,表面电阻R□至少降低10%,使R□低于6Ω/□,甚至低于2.1Ω/□,特别是大约1.9Ω/□。
由此,这样的基材对于制造低发射性或阳光控制的窗玻璃或具有高电导的半透明元件是特别有利的,比如等离子体显示装置的电磁防护屏。
在这些基材中,可以在银层上面沉积其它的电介质层。它们可以基于如上所述的氧化物或氮化物或氮氧化物选择。其本身可以或不可以曝露在离子束下进行沉积。
叠层可以包括至少两层银层,甚至于三层或四层银层。
按照本发明能够制造的叠层的例子包括如下顺序的各层:
…ZnO(i)/Ag/氧化物如ZnO…
…Si3N4/ZnO(i)/Ag/氧化物如ZnO…
…Si3N4/ZnO(i)/Ag/Si3N4/(任选的氧化物)…
…Si3N4/ZnO(i)/Ag/Si3N4/ZnO(i)/Ag/Si3N4…
…Si3N4/ZnO(i)/Ag/Si3N4/ZnO(i)/Ag/Si3N4/(氧化物)…
在此(i)指出该层是曝露在离子束下的,而且在至少一个银层的上面和/或下面可以插入金属阻隔层。
使用的基材也可以是塑料材料,特别是透明塑料材料。
本发明的另一个目的是如上所述基材的制造方法,即沉积叠层的方法,在该方法中,在雾化容器中,在曝露在至少一种来自离子源的离子束的条件下,通过阴极雾化,特别是磁场辅助和优选在氧和/或氮存在下的反应性的阴极雾化,在基材上沉积至少一层电介质层。按照本发明的方法,从线性离子源产生离子束,能够根据离子源的参数来调节曝露在离子束下的所述电介质层的折光指数。
如此就能够相对于没有离子束时沉积的此层的指数降低或增大曝露在离子束下的电介质层的折光指数。
有利的是,对于至少一部分可被沉积的电介质材料,无论指数如何变化,都通过曝露在离子束下来保持由阴极雾化而沉积在基材上的电介质层的密度。
在雾化室中曝露在离子束下的操作是与通过雾化沉积该层同时和/或相继进行的。
所谓“同时”,意味着电介质薄层的构成材料在受到离子束作用的时候,沉积还没有完全完成,即还没有达到其最终的厚度。
所谓“相继”,意味着电介质薄层的构成材料在受到离子束作用的时候,沉积已经完全完成,即在已经达到其最终厚度之后。
在与沉积的同时进行曝露的实施方案中,优选对一个或多个离子源的位置进行优化,使得来自靶的雾化颗粒的密度的最大值与一个或多个离子束相并列(juxtapose)。
为了制造基于氧化物的电介质层,优选以在离子源中非常主要是氧气,特别是100%氧气建立氧离子束,此时在雾化阴极上的气氛优选由100%的氩气组成。
在此实施方案中,在离子束下的曝露与通过雾化沉积该层同时进行。为此不需要像在先有技术中一样限制离子的能量,反之,有利的是建立能量为200~2000eV,甚至是500~5000eV,特别是500~3000eV的离子束。
可以将离子束直接引向基材和/或雾化阴极,特别是基材和/或阴极方向或与基材面和/或阴极的面分别不是0°角,使得离子束与通过雾化从靶上释放出的中性粒子流并行。
相对于在比如阴极中心的垂直方向测量的基材法线(normale)方向,特别是当阴极是圆柱形时,是在阴极轴线的垂直方向上,此角度可以为约10~80°。
在粒子流指向靶子的时候,来自离子源的离子束与通过雾化而形成的靶子“轨迹”是并行的,这就是说分别来自阴极和离子源的两个束的中心在基材的面上相遇。
也可以有利地使用在轨迹之外而朝向阴极的离子束,以增加靶子的使用率(侵蚀)。此时离子束可以以相对于通过阴极中心,特别是当阴极是圆柱形时通过其轴线的基材法线成±10~80°角指向雾化阴极。
在相继或同时的结构形状中,离子源与基材的距离是5~25cm,优选是10±5cm。
按照基材行进的方向,离子源可位于雾化阴极之前或之后(即在离子源与阴极或基材之间相对于通过阴极中心的基材法线的角是负的或正的)。
在本发明的一个实施方案中,在雾化容器中,在与雾化而沉积电介质层的同时由线性离子源建立离子束,然后用至少另一个离子束对沉积的层进行补充的处理。
通过详细阅读下面的非限定性实施例和说明按照本发明的装置的纵向剖面的图1将能更好地理解本发明。
为了制造所谓“功能”窗玻璃(日光控制的、低发射的、加热的…等),通常在基材上沉积包括至少一个功能层的薄层的叠层。
当此一个或几个功能层特别是基于银的层时,需要沉积其电子电阻和/或常规发射性都最小的银层(其厚度为8~15nm)。
为此,已知应该在氧化锌底层上沉积此银膜:
完好结晶锌的(i)(纤锌矿相),优选具有由与基材平行的基面(0002平面)构成的取向。
完好平滑的(ii)(最小粗糙度)。
现有的能够沉积氧化锌的技术方案不能同时得到这两个特征。
比如:
—这些解决方案能够使氧化锌结晶(加热基材。增大阴极的功率、增加厚度、增加氧的含量),但导致该层粗糙度增大,这就导致在上面沉积的银层性能明显变差。
—这些解决方案能够沉积出粗糙度很小或没有粗糙度的氧化锌(在低压下沉积、在很薄的厚度上沉积),但导致银层部分无定形化,这就改变了在ZnO上银的异质外延生长的质量。
在本发明中,已惊奇地发现沉积,特别是氧化锌以及很多其它电介质层的沉积在来自线性源的离子来的辅助下,在一定条件下可以沉积高度结晶的层,其具有很小的粗糙度。这使得明显改善了外延银层在下面的电介质层上的质量,并因此改善了叠层的光学和机械性能。
参考例1
在此例子中,借助于在图1中说明的装置(10),在玻璃基材上涂布40nm厚的氧化锌层。
此沉积装置包括处于真空下的雾化室(2),在其中在图中未显示的传送装置上,按照在图中箭头F所表示的方向和指向,使基材(1)行进。
此装置(2)包括磁场辅助雾化阴极(5)系统。此系统包括至少一个旋转的圆柱状(但它也可以是平面状的)阴极,它基本上在基材的整个宽度上展开,阴极的轴线基本上与基材相平行。此雾化阴极(5)系统定位在基材以上265mm的高度H5处。
从雾化系统的阴极释放出的物质被基本上成束(6)地射向基材。
此装置(2)还包括发射离子束(3)的线性离子源(4),该离子源基本上在基材的整个宽度上展开。此线性离子源(4)位于离阴极的轴线170mm的距离L4处,相对于基材的行进方向在阴极的前面,还位于基材以上120mm的高度H4处。
相对于通过阴极轴线的基材垂直线,离子束(3)具有角度A的取向。
使用已知的阴极雾化技术,在雾化容器(2)中,在含有氩和氧的气氛中,在行进在旋转型阴极前面的基材(1)上,在含有大约2wt%铝的Zn的基础上进行此沉积。行进的速度为至少1m/min。
报道在下面表1a中的沉积条件适合于建立低于化学计量量的氧化锌层,其折光指数为1.88(而化学计量量的氧化锌层具有1.93~1.95的折光指数)。
用X射线反射分光法对此层进行分析,以确定其密度、厚度,用X射线衍射法确定其结晶度。光谱在2θ=34°显示出典型的ZnO峰(0002)。用传统的Scherrer公式和使用基础参数从衍射光谱推导出雏晶尺寸。
还测量了透过此基材的光线透过率、由此基材反射的光线反射率和每平方电阻。测量的值都报道在下面的表1b中。
实施例1
在此实施例中,按照本发明在玻璃基材上涂布厚度40nm的氧化锌层。
在与参考例1中同样的雾化容器中,在只含有氩气的雾化阴极气氛中,在行进的基材上,由雾化阴极进行此沉积。使用位于雾化室中的线性离子源,与雾化同时从含有100%氧气的组合源中的气氛建立离子束。离子源是倾斜的,使得离子束以30°的角度指向基材。
经过改变的沉积条件,使得能够制造出折光指数为1.88的氧化锌层,其密度与参考材料是一样的。
在离子束中的曝露只对光学性能有小的影响。
X射线衍射光谱显示出很强的ZnO峰(0002),这表明ZnO的厚度是恒定的,结晶和/或取向明显的ZnO的量增加。
用SIMS测量的铁含量小于1%(原子)。
用Rutherford后散射法测量出,ZnO含有0.45%(原子)的氩。
表1a
雾化 | 离子源 | ||||||
压力 | 功率 | Ar | O2 | 能量 | Ar | O2 | |
单位 | μbar | kW | sccm | sccm | eV | sccm | sccm |
参考例1 | 0.8 | 3.0 | 80 | 70 | - | - | - |
实施例1 | 0.9 | 3.0 | 100 | 0 | 2000 | 0 | 80 |
表1b
性能 | |||||||
密度 | 指数 | TL | RL | R□ | 雏晶尺寸ZnO(nm) | ||
单位 | g/cm3 | % | % | Ω/□ | Scherrer | 基础参数 | |
参考例1 | 5.30 | 1.88 | 83.8 | 16.1 | ∞ | 17 | 15 |
实施例1 | 5.30 | 1.54 | 88.9 | 9.8 | ∞ | 12 | 12 |
实施例2
在此实施例中,在玻璃基材上制造如下的叠层:
10nm的ZnO/19.5nm的Ag/10nm的ZnO
在此,如在曝露在离子束下的实施例1那样得到下氧化锌层。
通过在雾化室中将基材停留适当的时间,以得到厚度减至10nm的氧化物层,如在实施例1制造出下层。
然后,在由100%的氩组成的气氛下,将基材在银的阴极之前行进,然后在参考例1的条件下,在氩和氧的气氛下重新在锌的阴极前行进。
用X射线衍射分析对此叠层进行分析,以确定其结晶状态。光谱在2θ=34°显示出典型的ZnO峰,在2θ=38°显示出典型的Ag峰。通过传统的Scherrer公式和使用基础参数从光谱推导出银雏晶的尺寸。
还测量了透过此基材的光线透过率、由此基材反射的光线反射率和表面电阻。
结果都报道在下面的表2中。
将此性能与没有曝露在离子束下制造的下氧化锌层的参考例2进行比较。
比较显示出,当使用离子束进行曝露制造出下面的氧化锌层时,银层的结晶得到明显的改善,这表现为表面电阻更小,或者是导电性得到改善。
表2
性能 | |||||
TL | RL | R□ | 雏晶尺寸Ag(nm) | ||
单位 | % | % | Ω/□ | Scherrer | 基础参数 |
参考例2 | 52.3 | 45.5 | 2.07 | 15.7 | 15.3 |
实施例2 | 58.6 | 40.7 | 1.86 | 17.4 | 17.6 |
参考例3
在此比较例中,在玻璃基材上制造如下的叠层:
基材 | SnO2 | TiO2 | ZnO | Ag | NiCr | SnO2 |
15 | 8 | 8 | 10 | 0.6 | 30 |
在此,如在实施例1用离子束进行曝露,得到下氧化锌层。
将基材在雾化室中停留适当的时间,以得到减至8nm厚度的氧化物层,如在实施例1操作制造氧化锌层。
然后在100%氩的气氛下使基材行进在银阴极之前。
单层窗玻璃(SV)和双层窗玻璃(DV4/15/4,其内部由90%的氩构成)的参考例3的光学性能和性质都显示在下面的表3中。
实施例3
此实施例在与参考例3同样的沉积条件下进行,只是在雾化室中装有线性离子源,并在用具有100%的氧源的气氛下制造氧化锌基的层时,用其在与雾化同时形成离子束。离子源是倾斜的,使离子束与基材成30°角,与基材的距离为大约14cm。
此改变的沉积条件能够形成折光指数基本上与参考层相等的氧化锌层。
单层窗玻璃(SV)和双层窗玻璃(DV4/15/4,其内部由90%的氩构成)的参考例3的光学性能和性质也显示在下面的表3中。。
表3
TL(%) | RL(%) | a* | b* | εn(%) | R□Ω/□ | ||
参考例3 | SV | 86 | 4.4 | 3.7 | -7.8 | ||
参考例3 | DV | 77.4 | 11.6 | 0.7 | -3.8 | 5.5 | 5 |
实施例3 | SV | 86.5 | 4.2 | 3.2 | -7.7 | ||
实施例3 | DV | 77.7 | 11.5 | 0.5 | -3.8 | 4 | 4.5 |
正如可以显示出的,光学性能仅受离子束曝露很少的影响,而热性能则明显地改善,因为在每平方电阻(R□)和正常发射性率(εn)方面得到10%的增益。
参考例4
在玻璃基材上制造如下厚度的叠层(单位:nm),这相当于SaintGobain Glass France公司商品名Plaistar的商品叠层:
基材 | SnO2 | ZnO | Ag | Ti | ZnO | Si3N4 | ZnO | Ag | Ti | ZnO | Si3N4 |
25 | 15 | 9.0 | 1 | 15 | 56 | 15 | 13.5 | 1 | 15 | 21 |
双层窗玻璃(4/15/4,其内层由90%的氩构成)的参考例4的光学性能和性质显示在下面的表4中。
实施例4
在与参考例4相同的条件下制造厚度与参考例4相同的叠层,只是在雾化室中设有线性离子源,并在制造与每一个银基功能层在下面直接相邻的每一层氧化锌基层时,用其与雾化的同时形成离子束。
在离子源处的气氛由100%的氧构成。离子源是倾斜的,使离子束以30°的角指向基材,与基材的距离为约14cm。每次通过时的离子束的能量为大约1000eV。在第一次通过时,雾化室内的压力为0.1μbar,第二次时为4.3μbar,在第一次通过时靶的功率是5.5kW,第二次通过时为10kW。
这样改变的沉积条件使得能够制造出折光指数基本上与参考层相同的氧化锌层。
双层窗玻璃(4/15/4,其内层由90%的氩构成)的实施例4的光学性能和性质也显示在下面的表4中。
正如可以显示出的,光学性能仅受离子束曝露很少的影响,而热性能则明显地改善,因为在每平方电阻(R□)方面得到10%的增益。
表4
TL(%) | λd(nm) | pe(%) | Rext(%) | L* | a* | b* | F.S.(CEN) | UW/m2·K | R□(Ω/□) | |
参考例4 | 71.8 | 553 | 2.6 | 12.0 | 41.2 | -2.3 | -1.7 | 42 | 1.17 | 2.7 |
实施例4 | 72.7 | 540 | 1.9 | 11.4 | 40.2 | -2.7 | -1.2 | 42 | 1.12 | 2.4 |
实施例5
沉积叠层:玻璃/Si3N4/ZnO(25nm)/Ag(9nm),然后测量氧化锌的结晶学特征和银层的电学特征。再评估没有被银覆盖和与前面同样的条件下制造的玻璃/ZnO(25nm)的RMS粗糙度。离子源相对于基材的倾角是30°。各测量的值显示在下面的表5中。
表5
Bragg0002(ZnO)峰的面积(u.a.) | 由AFM测量的RMS粗糙度(nm)厚度25nm | 9nm厚银膜的每平方电阻 | |
没有离子辅助的ZnO | 0 | 1.8 | 8.2 |
U=1500V | 78 | 1.4 | 7.0 |
U=3000V | 19 | 1.4 | 6.8 |
如此意外地观察到,使用离子束辅助沉积ZnO能够在如上所述的叠层中减小如此沉积的层的粗糙度。
实施例6
使用或不用离子束辅助的方法在玻璃上沉积单层的TiO2,然后通过模拟光学特征(分散的关系)和X射线反射的方法测量粗糙度。离子源相对于基材的倾角A是20°。测量的值显示在下面的表6中。
表6
光学粗糙度(nm) | X射线粗糙度RMS(nm) | |
无离子束辅助的TiO2 | 1.7 | 1.5 |
U=1000V | 0 | 0.5 |
U=2000V | 0 | 0.7 |
在前面以实施例的形式说明了本发明。但应该理解只要不偏离权利要求所定义的本专利的范围,本领域技术人员同样可实施本发明的各种实施方案。
Claims (31)
1.基材,特别是玻璃基材,其涂布有至少一层电介质薄层,该薄层通过阴极雾化,特别是磁场辅助和优选在氧和/或氮存在下的反应性的阴极雾化,通过曝露在至少一种来自于离子源(4)的离子束(3)下沉积,其特征在于,曝露在离子束下的所述电介质层是结晶的。
2.按照权利要求1的基材(1),其特征在于,通过曝露在离子束下由阴极雾化而沉积在基材上的所述电介质层具有很小的粗糙度。
3.按照权利要求2的基材(1),其特征在于,在离子束下的电介质层具有的粗糙度比不曝露在离子束下的同样电介质层的粗糙度小至少20%。
4.按照前面各项权利要求中任何一项的基材(1),其特征在于,所述电介质层是由化学计量量或非化学计量量的金属氧化物或氧化硅,或者由金属或硅的氮化物或氮氧化物形成的。
5.按照前面各项权利要求中任何一项的基材(1),其特征在于,所述电介质层是由下面当中的至少一种元素的氧化物形成的:硅、锌、钽、钛、锡、铝、锆、铌、铟、铈、钨。
6.按照权利要求5的基材(1),其特征在于,该层由氧化锌形成,其折光指数小于或等于1.95,特别是1.35~1.95。
7.按照权利要求5或6的基材(1),其特征在于,该层由氧化锌形成,其结晶度高于90%,特别是高于95%。
8.按照权利要求1~4中任何一项的基材(1),其特征在于,所述电介质层是由氮化硅或氮氧化硅形成的。
9.按照前面各项权利要求中任何一项的基材(1),其特征在于,所述层的氩含量为大约0.2~0.6%(原子)。
10.按照前面各项权利要求中任何一项的基材(1),其特征在于,所述层的铁含量小于或等于3%(原子)。
11.按照前面各项权利要求中任何一项的基材(1),其特征在于,该基材涂有叠层,其中的银层被沉积在所述曝露于离子束的电介质层的上面。
12.按照权利要求11的基材(1),其特征在于,在该银层的上面沉积另一层电介质层。
13.按照权利要求11或12的基材(1),其特征在于,该叠层包括至少两个银层。
14.按照权利要求11~13中任何一项的基材(1),其特征在于,其表面电阻R□小于6Ω/□,甚至小于2.1Ω/□,特别是为大约1.9Ω/□。
15.包括至少一按照前面各项权利要求中之一项的基材(1)的窗玻璃,特别是双层窗玻璃或夹层窗玻璃。
16.在基材(1)上沉积的方法,在该方法中通过阴极雾化,特别是磁场辅助和优选在氧和/或氮存在下的反应性的阴极雾化,在曝露在来自离子源(4)的至少一种离子束(3)的条件下,在雾化室(2)中,在该基材上沉积至少一层电介质薄层,其特征在于,在雾化室中形成离子束,其特征还在于,使曝露在离子束下的所述电介质层发生结晶。
17.按照权利要求16的方法,其特征在于,形成氧离子束。
18.按照权利要求16或17的方法,其特征在于,形成的离子束的能量为200~2000eV,甚至于为500~5000eV。
19.按照权利要求16~18中任何一项的方法,其特征在于,在曝露在离子束下的条件下通过阴极雾化在基材上沉积的所述电介质层具有很小的粗糙度。
20.按照权利要求16~19中任何一项的方法,其特征在于,曝露在离子束下的操作与通过雾化而沉积层的操作是同时进行的。
21.按照权利要求16~20中任何一项的方法,其特征在于,曝露在离子束下的操作与通过雾化而沉积层的操作是相继进行的。
22.按照权利要求16~21中任何一项的方法,其特征在于,离子束指向该基材(1),特别其指向的方向使得与该基材的表面形成非0的角度,优选在与该基材的表面形成10~80°的角度。
23.按照权利要求16~22中任何一项的方法,其特征在于,离子束指向至少一个阴极,特别其指向的方向使得与该阴极的表面形成非0的角度,优选在与该阴极的表面形成10~80°的角度。
24.按照权利要求16~23中任何一项的方法,其特征在于,从线性的源形成离子束。
25.按照权利要求16~24中任何一项的方法,其特征在于,在所述电介质层上沉积至少一层特别是基于银的功能层,其特征还在于,使所述功能层发生结晶。
26.按照权利要求25的方法,其特征在于,该银层的雏晶尺寸增大大约30~40%。
27.按照权利要求16~26中任何一项的方法,其特征在于,该电介质层是基于氧化锌的。
28.按照权利要求16~27中任何一项的方法,其特征在于,在与通过雾化沉积层的同时,从线性离子源(4),在雾化室(2)中形成离子束(3),然后用至少另外一个离子束对沉积的层进行补充的处理。
29.在基材(1)上,特别是在玻璃基材上进行沉积,用来制造按照权利要求1~14中任何一项的基材,或者实施按照权利要求16~28中任何一项方法的装置(10),该装置包括雾化室(2),在其中通过阴极雾化,特别是通过磁场辅助和优选在氧和/或氮存在下的反应性的阴极雾化,在曝露在至少一种离子束(3)的条件下在该基材上沉积至少一层电介质薄层,该装置的特征在于,在雾化室(2)中包括至少一个能够形成至少一种离子束的线性离子源(4)。
30.按照前面的权利要求的装置(10),其特征在于,线性离子源的位置使得离子束指向该基材,特别是在与该基材的表面形成非0角度,优选形成10~80°角度的方向上。
31.按照权利要求29或30的装置(10),其特征在于,线性离子源的位置使得离子束指向至少一个阴极,特别是在与该阴极的表面形成非0角度,优选形成10~80°角度的方向上。
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-
2003
- 2003-06-27 FR FR0307847A patent/FR2856677B1/fr not_active Expired - Fee Related
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2004
- 2004-06-28 EP EP04767496A patent/EP1641720A2/fr not_active Withdrawn
- 2004-06-28 CN CNA2004800247174A patent/CN1845882A/zh active Pending
- 2004-06-28 WO PCT/FR2004/001651 patent/WO2005000758A2/fr active Application Filing
- 2004-06-28 KR KR1020057025069A patent/KR101343437B1/ko not_active IP Right Cessation
- 2004-06-28 JP JP2006516335A patent/JP5026786B2/ja not_active Expired - Fee Related
- 2004-06-28 US US10/562,121 patent/US20060275612A1/en not_active Abandoned
- 2004-06-28 WO PCT/FR2004/001652 patent/WO2005000759A2/fr active Application Filing
- 2004-06-28 US US10/562,451 patent/US7820017B2/en not_active Expired - Fee Related
- 2004-06-28 CN CNA2004800247282A patent/CN1842500A/zh active Pending
- 2004-06-28 EA EA200600113A patent/EA012048B1/ru not_active IP Right Cessation
- 2004-06-28 JP JP2006516336A patent/JP2007519817A/ja not_active Withdrawn
- 2004-06-28 EA EA200600112A patent/EA011247B1/ru not_active IP Right Cessation
- 2004-06-28 EP EP04767497A patent/EP1641721A2/fr not_active Withdrawn
- 2004-06-28 KR KR1020057025068A patent/KR101172019B1/ko not_active IP Right Cessation
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2005
- 2005-12-21 ZA ZA2005/10376A patent/ZA200510376B/en unknown
- 2005-12-22 ZA ZA2005/10416A patent/ZA200510416B/en unknown
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2010
- 2010-09-07 US US12/876,625 patent/US20110056825A1/en not_active Abandoned
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2011
- 2011-07-29 JP JP2011166621A patent/JP2011241480A/ja active Pending
- 2011-07-29 JP JP2011167008A patent/JP2011241481A/ja active Pending
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Publication number | Publication date |
---|---|
ZA200510376B (en) | 2006-12-27 |
KR101172019B1 (ko) | 2012-08-08 |
WO2005000758A3 (fr) | 2005-10-13 |
KR101343437B1 (ko) | 2014-03-04 |
EP1641721A2 (fr) | 2006-04-05 |
FR2856677A1 (fr) | 2004-12-31 |
US7820017B2 (en) | 2010-10-26 |
JP2011241480A (ja) | 2011-12-01 |
EP1641720A2 (fr) | 2006-04-05 |
WO2005000759A3 (fr) | 2006-04-20 |
CN1845882A (zh) | 2006-10-11 |
WO2005000758A2 (fr) | 2005-01-06 |
US20060275612A1 (en) | 2006-12-07 |
KR20060026448A (ko) | 2006-03-23 |
JP2011241481A (ja) | 2011-12-01 |
EA012048B1 (ru) | 2009-08-28 |
EA011247B1 (ru) | 2009-02-27 |
KR20060036403A (ko) | 2006-04-28 |
ZA200510416B (en) | 2006-12-27 |
JP2007519817A (ja) | 2007-07-19 |
WO2005000759A2 (fr) | 2005-01-06 |
JP5026786B2 (ja) | 2012-09-19 |
EA200600113A1 (ru) | 2006-06-30 |
FR2856677B1 (fr) | 2006-12-01 |
US20060234064A1 (en) | 2006-10-19 |
US20110056825A1 (en) | 2011-03-10 |
EA200600112A1 (ru) | 2006-06-30 |
JP2007516341A (ja) | 2007-06-21 |
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