CN101415652A - 用于透明基材的高度耐热的具有低发射性多层体系 - Google Patents
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Abstract
本发明涉及用于透明基材的,尤其用于窗玻璃的高度耐热处理的低发射性多层体系,该体系包括,从基材开始,至少的由多个部分层组成的且包括与银基功能层相邻的主要由ZnO组成的一个层的下部抗反射性涂层,位于银-基层的顶部上的主要含金属的封闭层,由多个部分层组成的上部抗反射涂层以及任选由多个部分层组成的覆盖涂层。该上部抗反射涂层具有:用ZnO或用含有ZnO的或含有ZnO:Al/ZnMeOx型的混合氧化物的相继的层的混合氧化物ZnMeOx所制成的部分层;Si3N4或SixOyNz的部分层;和在这两个部分层之间,由具有立方晶格的金属氧化物或混合氧化物组成的具有0.5-5nm厚度的分离层,它防止在这两个部分层之间的直接接触。根据本发明,插入的分离层使得有可能进一步改进多层体系的机械和化学性质并获得高度耐技术装卸作业的有涂层的窗玻璃。
Description
本发明涉及用于透明基材的,尤其用于窗玻璃(vitres)的高度耐热处理的具有低发射性(émissivité)多层体系,该体系具有,从基材开始,至少一层具有下部抗反射性涂层(revêtement antirefletinférieur),该涂层由多个部分层(plusieurs couches partielleset)组成且包括与银-基功能层相邻的主要由ZnO组成的一个层,位于银-基层的顶部上的主要含金属的封闭层(couche métallique de blocage),由多个部分层组成的上部抗反射涂层(revêtement antireflet supérieur)以及任选由多个部分层组成的覆盖涂层(couche de recouvrement),这些层通过真空溅射施涂。
本发明还涉及引入了带有本发明的多层体系的至少一种基材的玻璃窗。
该表达短语“高度耐热的多层体系”被理解为指承受约600-750℃的温度的多层体系,这一温度是在没有破坏和损失玻璃基板的主要性能(即在可见谱区中的高透射率,在热辐射范围中的高反射率,低的色散,高的颜色中性,高的机械强度和高的耐化学性)的情况下弯曲和/或淬火(trempe)玻璃基板的操作所需要的。在窗玻璃(这些优选被沉积在它之上)的后续技术处理中,这些多层体系也称作“可淬火的(trempables)”和/或“可弯曲的(bombables)”体系。根本上,当然还有可能将这些多层体系沉积在没有随后热处理的基材上。因此,这些已知的多层体系和根据本发明的多层体系也适合于合成材料透明基材。
该术语“功能层”一般指能够固有地用于热绝缘(热反射性)的金属层。在很多情况下,目前的多层体系的功能层是以银为基础的或主要由银(它对多层体系的颜色中性具有积极影响)组成,但是其它材料也已知用于功能层,例如金和铜。
高度耐热的多层体系的各种实例是已知的。在第一组的高度耐热的多层体系中,抗反射层全部由氮化硅(Si3N4)组成,它通过由CrNi和/或NiCrOx组成的薄的封闭层与银功能层分隔开。
具有这些结构的多层体系例如已描述在文件EP 0 567 735 B1,EP 0 717 014 B1,EP 0 771 766 B1,EP 0 646 551 B1,EP 0 796 825 B1,EP 1 446 364 B1和EP 1 174 397 A2中。在文件EP 0 883 584 B1中描述的多层体系中,放置在镀银层和Si3N4抗反射层之间的封闭层由硅组成。
在有镀银层作为功能层的高度耐热的另一组多层体系中,该抗反射层由氧化物层组成。这些多层体系(其中抗反射层由纯氧化物组成)例如已描述在文件DE 198 52 358 C1,EP 0 991 92 B1,EP 1 538 131 A1和WO 2004/058660 A1中。这些多层体系也可提供有由金属氮化物(尤其Si3N4)组成的上层。
文件EP 0 718 250 B1教导了提供有氧化物、氮化物或碳化物抗反射层的可淬火的多层体系,其中银基功能层被金属封闭层覆盖,该封闭层例如由Nb,Ta,Ti,Cr或Ni或这些金属中的至少两种的合金组成。在一个实施方案中,薄的ZnO中间层被放置在位于镀银层上的Nb封闭层与Si3N4上部抗反射层之间。
文件DE 102 35 154 B4公开了一开始所指明的并提供有封闭层(以钛合金为基础)的那一类型的高度耐热的多层体系。该文件也描述了多层体系,其中任选Al-掺杂的ZnO层被施涂于金属封闭层,Si3N4层,它形成了上部抗反射涂层的一部分,象ZnO层位于这一ZnO层上。
文件DE 101 05 199 C1教导了提供有氧化物抗反射层的高度耐热的多层结构,在该结构中金属氮化物例如Si3N4或AlN的具有0.5-5nm厚度的中间层被放置在银层与位于银层顶部上的金属封闭层之间。
文献EP 1 238 950 A2和文献EP 1 583 723 A1描述了任选地具有多个银功能层和氮化物抗反射层或构成该抗反射层的氮化物部分层的可淬火多层体系,和其中相继的NiCrOx/SnO2/Si3N4层位于银功能层的顶部上。
文件DE 103 51 616 A1,它也涉及高度耐热的多层体系,也公开了具有相继多个层的多层体系:Ag/Si3N4/ZnO/SnO/Si3N4。
文献WO 97/48649也描述了提供有银功能层和Si3N4抗反射层的高度耐热的多层体系。根据该文件,位于银上层的顶部之上的相继多个层也由Nb/ZnO/TiN/Si3N4组成。
不仅关于耐热性而且关于机械和化学性能的严格要求都强加于可淬火或可弯曲的多层体系。在窗玻璃的公司内运输,裁切和打磨的过程中,在洗涤机中的洗涤过程中,在穿过淬火和/或弯曲炉的运输过程中和在后续的运输和处理操作(下面统称“装卸作业”)过程中,这些层暴露于高应力,容易地导致该多层体系的损害。
本发明的根本问题是进一步改进高度耐热的多层体系的机械和化学性能以及开发能够显示出良好的光学性质和高度耐技术性装卸作业(résistance aux manipulations techniques)的多层体系。
本发明用描述在权利要求1中的技术方案来解决这一问题。从属权利要求更详细地描述特别有利的特征。
虽然由于具有在银层顶部已知相继有Si3N4-ZnO的和/或在银层顶部的多层体系而基本上可能早已获得的较高硬度和良好装卸性能,由于有这些相继的层,故有时会观察到在后续的生产和处理操作中有质量缺陷。令人吃惊地,这些质量缺陷可以通过,根据本发明,插入由金属氧化物或具有立方晶格的混合氧化物制成的分离层来避免。
相继的Si3N4-ZnO和ZnO-Si3N4层的敏感性的一个原因是界面层(couche frontiere)建立的缺陷。这是因为Si3N4是具有突出各向同性的无定形物质,而ZnO是具有非常致密的六方堆积和各向异性的晶体材料。该各向异性是由晶格的空间结构所引起并且例如在弹性,硬度,剥离的能力和热伸长上表现出来,并且这也随着这些性能对于方向的依赖性而变化。然而,作为分离层被插入的具有立方晶格的晶体材料的层从光学观点看是各向同性的,但是就它的机械性能而言,它相当于各向异性材料。因此,它实现了两个功能和以这一方式用作能够增强在Si3N4层和ZnO层之间的粘结作用的一个层。
适合于具有立方晶格的分离层的材料的例子是以NiCrOx、Al2O3、MgAlOx TiAlOx、NiAlOx和NiO为基础或由NiCrOx、Al2O3、MgAlOx TiAlOx、NiAlOx和NiO组成的各层。含有ZnO的混合氧化物层能够以ZnSnOx,ZnAlOx,ZnBiOx,ZnSbOx或ZnInOx为基础或由ZnSnOx,ZnAlOx,ZnBiOx,ZnSbOx或ZnInOx组成(这是常见的,下标字母表示获得某化学计量的数值)。
由本发明所提出的上部抗反射涂层的各部分层的相继存在,即,由具有立方晶格的金属氧化物或混合氧化物制成的分离层在含有ZnO的部分层和,在本发明的有利发展中,氮化硅部分层之间的排列(agencement)选择性地或累积地能够在多层体系的下部抗反射性涂层内产生。因此,在权利要求1的前述部分的范围内有可能生产下部抗反射性涂层和/或上部抗反射涂层,它具有:
- 用ZnO或用含有ZnO的或ZnO:Al/ZnMeOx型的混合氧化物的相继的层的混合氧化物ZnMeOx所制成的部分层;
- Si3N4或SixOyNz的部分层;和
- 在这两个部分层之间,由具有立方晶格的金属氧化物或混合氧化物组成的具有0.5-5nm厚度的分离层,它防止在这两个部分层之间的直接接触。
根据本发明,该多层体系也特别具有下面给出的部分层的排列:
基材(玻璃)/Si3N4/ZnO:Al/Ag/NiCr/ZnO:Al/NiCrOx/Si3N4/(覆盖涂层);
基材(玻璃)/Si3N4/NiCrOx/ZnO:Al/Ag/NiCr/ZnO:Al/NiCrOx/Si3N4/(覆盖涂层);
基材(玻璃)/Si3N4/ZnSnOx/ZnO:Al/Ag/NiCr/ZnO:Al/NiCrOx/Si3N4/(覆盖涂层);
基材(玻璃)/Si3N4/NiCrOx/ZnSnOx/ZnO:Al/Ag/NiCr/ZnO/ZnSnOx/NiCrOx/Si3N4/(覆盖涂层)。
还有可能改进具有以某些TiZrHf化合物为基础的覆盖涂层的多层体系的机械强度性能。
第一有利的覆盖涂层(“topcoat”)由TiZrHf(CxOyNz)组成。这一覆盖涂层是从TiZrHf金属靶溅射的,其中添加了0.5%的CH4的N2气用作工作气体。然而,还有可能省去CH4的添加并且有可能利用在具有较低水平的吸入容量的泵吸系统中存在的烃类在包围TiZrHf靶的工作气体中获得所需的碳,这些内容也基本上公开在文件EP 0270 024 B1(其中TiCxOyNz层的溅射)中。紧接着当该层与大气接触时发生氧的引入。通过使用AES(俄歇电子能谱学)和XPS/ESCA(化学分析电子光谱法),已经有可能表明,所制备的覆盖涂层具有均匀的TiZrHf/碳氧化氮化物(carboxynitride)结构。此类结构的存在是在专业文献中已知的(例如参见the German journal Hochvakuum,
/Dünne Schichten,volume 1,March 1984,page 142和thejournal Thin Solid Films,100(1983),pages 193 to 201,entitled“Themicrohardness of reactively sputtered TiCxOyNzfilms”)。
文件WO 2004/71984 A1公开可淬火的多层体系,其中覆盖涂层可以由Ti、Zr以及元素周期表的IVb、Vb和VIb族的其它元素的氮化氧化物、碳化氧化物和碳氮化物组成。然而,这些已知的多层体系是各种化合物的混合物并且这一层不具有与在本发明中生产的复杂和均匀的粘结结构相同的结构。
另一种有利的覆盖涂层由纯TiZrHfYOx氧化层组成。这一氧化的覆盖涂层优选从含有5-10%(按重量)的Y2O3(相对于ZrO2含量)的氧化的导电陶瓷靶溅射的。这一层优选在Ar/O2工作氛围中从管式靶溅射的。
本发明现在借助于两个举例说明的例子来描述,它们与现有技术的对比实施例相比较。因为根据本发明的技术方案需要改进特别机械强度和硬度,评价在有涂层的窗玻璃上各层的性能,所以进行下面所指的测量和试验。
A.泰伯(Tabcr)试验(公司Taber Industries)
在本试验中,未淬火的有涂层的试样被夹在该装置中并且使用CS-10F型的摩擦辊来处理,在于让摩擦辊在500g的荷载下旋转50转。以这一方式处理的涂层在显微镜下进行评价。这一试验的结果表示为仍然存在的各层的百分比。
B.在未淬火的试样上的埃里克森划痕硬度试验
在5N的荷载下通过使用“van Laar”型的点,在该层中的尺寸10×10cm2的未淬火的有涂层的试样上产生圆形划痕。接着,该试样进行热淬火,在显微镜下测量划痕的宽度。划痕越窄,涂层受张力越少,涂层的质量越好。
C.在淬火的试样上的埃里克森划痕硬度试验
在尺寸10×10cm2的预应力试样上的涂层中,在递增的荷载下,在与试验B中相同的装置中产生圆形划痕,以及测定观察到中断划痕的荷载和观察到连续划痕的荷载。
D.在无预应力的试样上的埃里克森擦洗试验
无预应力的有涂层的试样进行根据ASTM 2486标准的埃里克森擦洗试验。这一试验测量到有可能在300个冲程之后在涂层中观察到缺陷的程度。
E.在预应力试样上的埃里克森擦洗试验
具有10×40cm2的尺寸的有涂层的试样在淬火炉中淬火并且进行相同的擦洗试验。测量开始观察到涂层的剥离时的冲程的数量。
F.由我们自己的试验方法测量抗划性
在本测量中,负载了一定重量的针在规定的速率下在涂层上划,在淬火之前(v)和在淬火(n)之后都如此。划痕的痕迹是可见的那一重量g是抗划性的量度。
G.钢毛试验
在本试验中,钢毛垫片在轻微压力下在未淬火试样的涂层上通过。当没有观察到划痕时,这被认为是通过该试验。
H.酒精试验
通过使用醇浸渍的抹布擦拭涂层,在施加预应力之后进行这一试验。没有看见摩擦斑点。
I.使用从公司Gardner获得的光散射测量装置的测量
I.1. 在(v)之前和在(n)淬火之后色散光的测量。
I.2.在(v)之前和在(n)淬火之后透射率的测量。
对比实施例
在工业连续涂敷装置中将与现有技术对应的低发射性多层体系施涂于4mm厚度的浮法玻璃的窗玻璃上,在该装置中有可能使用全部类型的靶,即平面靶和管式靶,在交流电和/或直流电条件下,通过使用反应活性磁控溅射(即由磁场维持的反应活性阴极溅射),在化学符号之前给出的数字表示各层的厚度(nm):
玻璃/25Si3N4/9ZnO:Al/11.5Ag/3.5NiCr/5ZnO:Al/33Si3N4/2Zn2TiO4。
ZnO:Al层是从含有2%Al(重量)的ZnAl金属靶溅射的。位于银层上的封闭层是在氩气作为工作气体的情况下从由80%Ni(重量)和20%Cr(重量)组成的NiCr金属靶溅射的。氮化硅上部抗反射层是在反应活性条件下以Ar/N2作为工作气体从Si靶溅射的,以及上部覆盖涂层(此层称为“topcoat”)也是在反应活性条件下以Ar/O2作为工作气体从由ZnTi合金(含有73% Zn(重量)和27% Ti(重量))组成的金属靶溅射的。进行上述试验所需要的试样从有涂层的窗玻璃上裁切的。
当试样需要施加预应力时,这是在符合该技术标准的从EFKO公司获得的47067型的高性能炉中进行的。
这些性能通过使用上述试验在对比实施例的试样上测定的:
A.泰伯试验: | 80% |
B.在埃里克森划痕硬度试验中划痕的宽度: | 160-180μm |
C.划痕的视觉评价: | 连续划痕1N |
D.在未淬火玻璃上的擦洗试验: | 在30次通过后涂层剥离的开始 |
E.在淬火玻璃上的擦洗试验: | 没有缺陷的涂层 |
F.抗划性: | (v):55-64g;(n):15-20g |
G.钢毛试验: | 划痕斑点 |
H.酒精试验: | 没有可见斑点 |
I1.光散射: | (v):0.17%;(n):0.30% |
I2.透射率: | (v):84%;(n):89% |
举例性实施例1
4mm厚度的浮法窗玻璃在与对比实施例中使用的相同的连续涂敷装置中涂覆下列多层体系:
玻璃/25Si3N4/9ZnO:Al/11.5Ag/3.5NiCr/5ZnO:Al/2.5NiCrOx/33Si3N4/2TiZrHf(CxOyNz)
ZnO:Al层、NiCr层和Si3N4层在与对比实施例所指定的相同条件下溅射而成。该NiCrOx层也从80/20NiCr层溅射,但是在反应性条件下,其中Ar/O2混合物(250/90cm3,在标准大气条件下)用作工作气体。该靶用于沉积由TiZrHf合金(它由55% Ti(重量),44%Zr(重量)和1% Hf(重量)组成)组成的TiZrHf(CxOyNz)覆盖涂层并在Ar和N2混合物作为工作气体的情况下被溅射涂覆。在降低在这一阴极上的抽吸力之后碳从该装置中所存在的残留气体中被引入到覆盖涂层中,并且氧也从该残留气体中引入,而且也可以在覆盖涂层已经与外部大气接触之后从大气中引入。在这一覆盖涂层上进行的XPS/ESCA和AES测量很好地对应于在文献中公开的Me-碳氧化氮化物结构中的数据。
使用上述试验在这一产物上测定下列性能:
A.泰伯试验: | 87% |
B.在埃里克森划痕硬度试验中划痕的宽度: | 80μm |
C.划痕的视觉评价: | 连续划痕7N |
D.在未淬火玻璃上的擦洗试验: | 在200次通过后涂层剥离的开始 |
E.在淬火玻璃上的擦洗试验: | 没有缺陷的涂层 |
F.抗划性: | (v):141-450g;(n):60-80g |
G.钢毛试验: | 没有可见斑点 |
H.酒精试验: | 没有可见斑点 |
I1.光散射: | (v):0.17%;(n):0.18% |
I2.透射率: | (v):74.4%;(n):87% |
在施加预应力之前试样的透射率(74.4%)是较低的,因为TiZrHf(CxOyNz)覆盖涂层是相对高度吸光性的。只是在淬火热处理操作之后氮化物和碳化物组分分解成无吸光性氧化物。
举例性实施例2
4mm厚度的浮法窗玻璃在与对比实施例中使用的相同的连续涂敷装置中涂覆下列多层体系:
玻璃/25Si3N4/2.5NiCrOx/9ZnO:Al/11.5Ag/3.5NiCr/5ZnO:Al/2.5NiCrOx/Si3N4/2TiZrHfYOx.
TiZrHFYOx覆盖涂层从由陶瓷(由导电性的氧化的材料组成)制成的管式靶沉积而成。该氧化的材料是从含有56% Ti(重量),40%Zr(重量),1% Hf(重量)和3% Y(重量)的金属合金制备的。其它层是在与前面实施例中相同条件下溅射而成。
使用上述试验在这一产物上测定下列性能:
A.泰伯试验: | 90% |
B.在埃里克森划痕硬度试验中划痕的宽度: | 50-60μm |
C.划痕的视觉评价: | 连续划痕10N |
D.在未淬火玻璃上的擦洗试验: | 在450次通过后涂层剥离的开始 |
E.在淬火玻璃上的擦洗试验: | 没有缺陷的涂层 |
F.抗划性: | (v):139-366g;(n):80-105g |
G.钢毛试验: | 没有可见斑点 |
H.酒精试验: | 没有可见斑点 |
I1.光散射: | (v):0.18%;(n):0.18% |
I2.透射率: | (v):84%;(n):87% |
在对有涂层的窗玻璃施加预应力后,这一多层体系当在日光下以一定的入射余角或在卤素灯光下观察时可再现地没有粗糙处和翳影(voile)。
Claims (11)
1.用于透明基材的,尤其用于窗玻璃的高度耐热处理的低发射性多层体系,该体系具有,从基材开始,至少一层下部抗反射性涂层,该涂层由多个部分层组成,包括与银-基功能层相邻的主要由ZnO组成的层,位于银-基层的顶部上的主要含金属的封闭层,由多个部分层组成的上部抗反射涂层以及任选由多个部分层组成的覆盖涂层,这些层通过真空溅射法施涂,其特征在于上部抗反射涂层具有:
-用ZnO或用含有ZnO的或ZnO:Al/ZnMeOx型的混合氧化物的相继的层的混合氧化物ZnMeOx所制成的部分层;
-Si3N4或SixOyNz的部分层;和
-在这两个部分层之间,由具有立方晶格的金属氧化物或混合氧化物组成的具有0.5-5nm厚度的分离层,它防止在这两个部分层之间的直接接触。
2.根据权利要求1所要求的多层体系,特征在于分离层是以NiCrOx,Al2O3,MgAlOx,TiAlOx,NiAlOx或NiO为基础或由NiCrOx,Al2O3,MgAlOx,TiAlOx,NiAlOx或NiO组成。
3.根据权利要求1和2中任何一项所要求的多层体系,特征在于含有ZnO的混合氧化物是以ZnSnOx,ZnAlOx,ZnBiOx,ZnSbOx或ZnInOx为基础或由ZnSnOx,ZnAlOx,ZnBiOx,ZnSbOx或ZnInOx组成。
4.根据权利要求1-3中一项的多层体系,特征在于用ZnO或用含有ZnO的或由ZnO:Al/ZnMeOx型的混合氧化物的相继的层组成的混合氧化物所制成的部分层被直接布置在金属封闭层上。
5.根据权利要求1-4中一项所要求的多层体系,特征在于该下部抗反射性涂层还具有:
-用ZnO或用含有ZnO的或ZnO:Al/ZnMeOx型的混合氧化物的相继的层的混合氧化物ZnMeOx所制成的部分层;
-Si3N4或SixOyNz的部分层;和
-在这两个部分层之间,由具有立方晶格的金属氧化物或混合氧化物组成的具有0.5-5nm厚度的分离层,它防止在这两个部分层之间的直接接触。
6.根据权利要求1-5中一项的多层体系,特征在于布置在上部抗反射涂层的顶部上的覆盖涂层由TiZrHf(CxOyNz)组成。
7.根据权利要求1-5中一项的多层体系,特征在于布置在上部抗反射涂层的顶部上的覆盖涂层由TiZrHfYOx组成。
8.根据前述权利要求中一项的多层体系,以下列层状结构为特征:基材/Si3N4/znO:Al/Ag/NiCr/ZnO:Al/NiCrOx/Si3N4/TiZrHf(CxOyNz)。
9.根据权利要求1-7中一项的多层体系,以下列层状结构为特征:基材/Si3N4/NiCrOx/ZnO:Al/Ag/NiCr/ZnO:Al/NiCrOx/Si3N4/TiZrHfYOx。
10.根据权利要求1-7中一项的多层体系,以下列层状结构为特征:基材/Si3N4/ZnSnOx/ZnO:Al/Ag/NiCr/ZnO:Al/NiCrOx/Si3N4/TiZrHf(CxOyNz)。
11.引入了根据前述权利要求中一项所要求的带有多层体系的至少一种基材的玻璃窗。
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CN114163142B (zh) * | 2021-11-23 | 2024-02-06 | 太仓耀华玻璃有限公司 | 一种磁控溅射单银low-e钢化玻璃及其制造工艺 |
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-
2006
- 2006-03-29 DE DE200610014796 patent/DE102006014796B4/de not_active Expired - Fee Related
-
2007
- 2007-03-28 JP JP2009502171A patent/JP5529528B2/ja not_active Expired - Fee Related
- 2007-03-28 EA EA200870383A patent/EA015326B1/ru not_active IP Right Cessation
- 2007-03-28 EP EP07731838A patent/EP2001813A2/fr not_active Withdrawn
- 2007-03-28 US US12/295,090 patent/US8043707B2/en not_active Expired - Fee Related
- 2007-03-28 CN CN2007800123512A patent/CN101415652B/zh not_active Expired - Fee Related
- 2007-03-28 CA CA 2647412 patent/CA2647412A1/fr not_active Abandoned
- 2007-03-28 WO PCT/FR2007/051032 patent/WO2007110552A2/fr active Application Filing
- 2007-03-28 BR BRPI0709920-7A patent/BRPI0709920A2/pt not_active IP Right Cessation
- 2007-03-28 KR KR1020087023853A patent/KR101400420B1/ko not_active IP Right Cessation
Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
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CN110506033A (zh) * | 2017-03-09 | 2019-11-26 | 佳殿玻璃有限公司 | 具有带有ir反射层和含铪的高折射率氮化电介质层的低e涂层的涂覆制品 |
Also Published As
Publication number | Publication date |
---|---|
DE102006014796A1 (de) | 2007-10-04 |
JP2009531266A (ja) | 2009-09-03 |
US8043707B2 (en) | 2011-10-25 |
EA200870383A1 (ru) | 2009-04-28 |
BRPI0709920A2 (pt) | 2011-07-26 |
KR20080106952A (ko) | 2008-12-09 |
WO2007110552A3 (fr) | 2007-11-15 |
WO2007110552A2 (fr) | 2007-10-04 |
EP2001813A2 (fr) | 2008-12-17 |
CA2647412A1 (fr) | 2007-10-04 |
KR101400420B1 (ko) | 2014-05-27 |
US20100178492A1 (en) | 2010-07-15 |
EA015326B1 (ru) | 2011-06-30 |
CN101415652B (zh) | 2013-03-13 |
DE102006014796B4 (de) | 2009-04-09 |
JP5529528B2 (ja) | 2014-06-25 |
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