CN101395096A - 被提供有热性能的叠层的基材 - Google Patents
被提供有热性能的叠层的基材 Download PDFInfo
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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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- C03C17/00—Surface treatment of glass, not in the form of fibres or filaments, by coating
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Abstract
本发明涉及一种基材(10),尤其是透明玻璃基材,被提供有一种薄膜叠层,该叠层包含具有在红外和/或目光范围反射性能的功能层(40),尤其是基于银或含银金属合金的金属功能层,以及2个涂层(20、60),所述涂层由多个介电层(24、26;64)组成,让每个功能层(40)位于2个涂层(20、60)之间,功能层(40)沉积在润湿层(30)上,润湿层本身分别直接沉积到下层涂层(20)上。本发明基材的特征在于,下层涂层(20)包含至少一个氮化物基的,尤其是氮化硅基的和或氮化铝基的介电层(24),和至少一个由混合氧化物制成的非结晶平滑层(26),所述平滑层(26)与所述上层润湿层(30)接触。
Description
本发明涉及透明基材,尤其是由刚性无机材料,如玻璃制成的那些,所述基材覆盖有薄膜叠层,该叠层包含能作用于日光和/或长波红外线的金属型功能层。
本发明更具体地说涉及此种基材用于制造热绝缘和/或防晒保护玻璃板(vitrage)的应用。这样的玻璃板可用于装备建筑物也可以装备车辆,尤其为了减少或防止由建筑物和乘用车厢内日益增长的玻璃表面的使用所带来的空调负荷和/或过度晒热(被称作“日光控制”玻璃的玻璃)和/或减少能量朝外部的散失(被称作“低-发射”玻璃的玻璃)。
这样的玻璃板另外还可被结合在具有特殊功能的玻璃,例如,加热玻璃或电致变色玻璃。
一种公知的赋予基材此类性能的叠层由具有在红外和/或日光范围中的反射性能的金属功能层组成,尤其基于银或含银金属合金的金属功能层。
该金属功能层以结晶形式沉积在润湿层上,后者也是结晶的,这有助于沉积在它上面的金属层的恰当结晶取向。
该功能层被置于2个由金属氧化物或氮化物型介电材料制成的涂层之间。该叠层通常通过系列沉积获得,该沉积通过采用真空技术,例如任选地磁场辅助的阴极喷镀进行。还可设置1,或甚至2个,非常薄的膜,叫做“阻隔涂层”,这个或这些涂层直接置于每个银基金属功能层的下面、上面或每一侧,当后面可能的对沉积物的热处理时,该下层涂层(revê tement sous-jacent)作为粘结层(rev ê tement d’accrochage)、成核层和/或保护层,和如果置于银基层上面的层在氧或氮气的存在下通过阴极喷镀进行沉积和/或如果叠层在沉积后经受热处理时,该上层涂层作为保护层或“牺牲层”以防止银受到损坏。
还可以从欧洲专利申请号EP 803 481已知的是,在基于氧化锌的层下方使用基于氧化锌的直接接触基材的无定形层。
已证明,当此种无定形层不是直接沉积到基材上,而是被插入到至少一个下层介电层与润湿层之间时,它可以改性介电层与位于其上的润湿层之间的界面并从而显著改善润湿层的结晶,同时也显著改善金属功能层的结晶。
现已惊奇地发现,将这样一种无定形层并入到在功能层下面并被提供有至少一个位于该无定形层下面的氮化物基介电层的涂层中可以达到功能层所要求的结晶改进并从而达到整个叠层电阻率的要求改进。
因此,本发明的目的是弥补现有技术的缺点,开发出一种具有上面描述的那些类型各层的新型叠层,该叠层具有比具有相似厚度的功能层和等效涂层的叠层更低的改善的电阻率,所述叠层经受或不经受1次(或多次)弯曲、钢化和退火类的高温热处理,而如果它经受1次(或多次)此类处理,完全保持其光学品质和机械完整性。
因此,本发明的目的,就其最广的公认意义而言,是一种基材,尤其是透明玻璃基材,其被提供有薄层叠层,该叠层包含具有在红外和/或日光范围反射性能的功能层,尤其是基于银或含银金属合金的金属功能层,以及2个涂层,所述涂层由多个介电层组成,使得功能层位于2个涂层之间,功能层沉积在润湿层上,该润湿层本身直接沉积到下层涂层上,特征在于,该下层涂层包含至少一个基于氮化物,尤其是氮化硅和/或氮化铝的介电层和至少一个由混合氧化物制成的非结晶平滑层,所述平滑层与所述上层润湿层相接触。
于是,本发明在于提供一种位于结晶的润湿层下方的非结晶平滑层,为了使位于该润湿层上面的功能层的恰当生长,该平滑层与润湿层直接接触或者通过下阻隔涂层(revêtement de sous-blocage)介质。
已发现,下层涂层包含至少一个基于氮化物,尤其是氮化硅和/或氮化铝的介电层的情况下,选择由混合氧化物制成的非结晶平滑层可以获得优良的叠层电阻率和符合预期的光学性能,不论基材是否在沉积后经受热处理。
因此,本发明还应用于所谓的“钢化或未钢化”的基材,例如,可以在建筑物同一正面上彼此靠近地布置结合有钢化的基材和未钢化基材的玻璃板,却不能借助对反射时颜色和光反射的简单肉眼观察将它们彼此区别开来。
就本发明的意义而言,当提到,某一层或涂层(包含1个或多个层)直接被沉积在另一沉积层之下或直接在其上时,指的是,在这两个沉积层之间不得有其他层插入。
平滑层在以下的意义上被称作为“非结晶的”:它们可以是完全无定形或者是部分无定形并因此部分结晶的,但它们不得在其整个厚度都完全是结晶的。它可以是金属性质的,因为它基于混合氧化物(混合氧化物是一种至少2种元素的氧化物)。
平滑层的结晶学外观必定区别于润湿层,因为平滑层是非结晶的,而润湿层基本上是结晶的;因此,从这一角度看它们不可能被混淆。
此种平滑层的优点是能获得一种不非常粗糙的、与直接在上面的润湿层之间的界面。这种低粗糙度还可用透射电镜进一步观察到。
再者,润湿层具有较好质地,另外还具有更明显的优选结晶取向。
因此,每个平滑层由不同于直接位于其上方的润湿层的材料组成,从结晶学和化学计量的角度都不同。
另外还包含平滑层的下层涂层的基于氮化物的层直接地或者通过接触层介质(例如,基于二氧化钛(TiO2))与基材接触。
该基于氮化物的层的指数优选地小于2.2。
优选地,平滑层是基于下列金属的一种或多种的氧化物的混合氧化物层:Sn、Si、Ti、Zr、Hf、Zn、Ga、In,更确切地说,是一种在低温沉积的基于锌和锡的混合氧化物的层或铟和锡混合氧化物(ITO)的层。
该平滑层的指数优选地小于2.2。
另外优选地,该平滑层是氧含量不符合化学计量式的混合氧化物层,更具体地说,还是基于以锑掺杂的基于亚化学计量的锌和锡的混合氧化物(SnZnOx:Sb,x是数字)层。
另外,平滑层优选地具有介于0.1~30nm的几何厚度,更优选0.2~10nm。
在优选的实施方案中,至少一个阻隔涂层基于Ni或Ti或基于一种镍基合金,尤其是基于NiCr合金。
另外,在功能层下面的润湿层优选基于氧化锌;该润湿层尤其可基于铝-掺杂的氧化锌。
润湿层的几何厚度优选介于2~30nm,更优选介于3~20nm。
本发明玻璃至少包括载有本发明叠层的基材,任选地与至少1个其他基材结合。每个基材可以是透明或着色的。其中至少一个基材尤其可由本体-着色的玻璃制成。着色类型的选择将取决于该玻璃一旦制造完成后对玻璃所要求的透光率和/或色度学外观。
因此,对用于装配车辆的玻璃板来说,例如,某些标准规定,挡风玻璃应具有约75%的透光率TL,而其他标准则要求约65%的透光率TL;例如侧窗或天窗则不要求这样的透光率水平。例如,可使用的着色玻璃是,在光源D65下,对于厚度4mm的而言,具有65%~95%的TL,40%~80%的透能率TE,470nm~525nm的主透射波长的玻璃,与0.4%~6%的透射纯度的结合,这可在色度体系(L,a*,b*)中通过分别介于-9~0之间和-8~+2之间的透射a*和b*值“表示(traduire)”。
就旨在装配在建筑物上的玻璃来说,对于“低-透射”应用,该玻璃优选地具有至少75%或更高的透光率TL,以及对于“日光控制”应用,至少40%或更高的透光率TL。
本发明玻璃板可具有层压结构,尤其通过至少1个热塑性聚合物片材结合了至少2个玻璃型刚性基材,从而具有以下类型的结构:玻璃/薄层叠层/1个或多个片材/玻璃。该聚合物尤其可基于聚乙烯醇缩丁醛PVB、乙烯/醋酸乙烯EVA、聚对苯二甲酸乙二醇酯PET或聚氯乙烯PVC。
该玻璃还可具有所谓不对称的层压玻璃板结构,它与玻璃型刚性基材与至少一个具有吸能性质的聚氨酯型聚合物片材结合,任选地与另一层具有“自愈合”性能的聚合物结合。有关此类型玻璃板的进一步细节可参见,尤其是专利EP-0 132 198、EP-0 131 523、EP-0 389 354。
因此,该玻璃具有以下类型的结构:玻璃/薄层叠层/聚合物片材。
本发明玻璃能经受热处理而不伤及薄膜叠层。因此,该玻璃可任选地被弯曲和/或钢化。
该玻璃,当由被提供有叠层的单一基材组成时,可以被弯曲和/或钢化。这时,它被称作“单块”玻璃。当该玻璃被弯曲,尤其为了构成用于车辆的玻璃板时,薄膜叠层优选地位于至少部分地非平面的面上。
该玻璃也可以是多(层)玻璃板,尤其是双层玻璃板,至少该载有叠层的基材是弯曲和/或钢化的。在多玻璃结构中优选的是,该叠层被置于面朝插入的气体层的的位置。在层压结构中,载有叠层的基材优选地与聚合物片材接触。
当该玻璃板是单块或呈双层玻璃板或层压玻璃板型的多层玻璃板形式时,至少该载有叠层的基材可由弯曲或钢化玻璃制成,该基材可在沉积叠层以前或以后进行弯曲或钢化处理。
本发明还涉及一种制造本发明基材的方法,它包括采用任选地磁场辅助的阴极喷镀型真空技术在其基材上沉积薄层叠层,随后对覆盖的基材实施弯曲、钢化或退火类型的热处理,而不会损害其光学和/或力学品质。
然而,并不排除叠层的1个或多个第一层可以利用其他技术进行沉积,例如,采用高温热解型热分解技术。
本发明的细节和优点特征通过以下借助于附图示出的非限制性实施例将变得更清楚。
图1示出了单功能层的叠层(有或没有平滑层)的薄层电阻在热处理前随着设置在下面的介电层厚度的变化,该叠层被提供有上阻隔单层涂层;
图2示出了与图1所示相同的单功能层的叠层(有或没有平滑层)的薄层电阻在热处理后随着位于其下的介电层的厚度的变化;
图3示出了单功能层的叠层的薄层电阻在热处理前随着平滑层的厚度的变化,其中该叠层被提供有单层阻隔涂层;
图4示出了与图3所示相同的单功能层的叠层的薄层电阻在热处理后随着平滑层厚度的变化;
图5示出了本发明的单功能层叠层,该功能层被提供有罩面上阻隔涂层但没有下阻隔涂层;
图6示出了本发明的单功能层叠层,该功能层被提供有下阻隔涂层但没有上阻隔涂层;以及
图7示出了本发明的单功能层叠层,该功能层被提供有下阻隔涂层并被提供有上阻隔涂层。
在这些示出多层叠层的附图中,为更容易理解,不同材料的厚度并未严格按照比例示出。
另外,在下面的所有实施例中,薄膜叠层被沉积在由钠钙玻璃制成的基材10上,基材厚度为2mm。
在对基材施加热处理的所有情况下,热处理是在约660℃温度进行约5min的退火处理,以及随后在环境空气(约20℃)中的冷却。
图1~4的目的是说明平滑层在示出本发明叠层的图5中示出的叠层类型的叠层中存在的重要性。
本发明的单功能的叠层的编号为1的实施例,是以下类型:
基材/Si3N4/SnZnOx:Sb/ZnO/Ag/Ti/ZnO/Si3N4
可变/可变/8nm/10nm/2nm/8nm/20nm
在图1和2中,曲线C1和C11分别示出了当叠层未被提供有平滑层时,分别在热处理之前(BHT)和之后(AHT),叠层的薄层电阻(Ω)随与基材接触的氮化硅(e Si3N4)基的介电层厚度的变化。
曲线C2和C12分别示出了当叠层被提供有6nm厚的由SnZnOx:Sb(x代表非零的数值)制成的平滑层时,分别在热处理之前和之后,叠层的薄层电阻(Ω)随与基材接触的氮化硅(e Si3N4)基的介电层厚度的变化。
曲线C3和C13分别示出了当叠层被提供有20nm厚的SnZnOx:Sb基的平滑层时,分别在热处理之前和之后,叠层的薄层电阻(Ω)随与基材接触的氮化硅(e Si3N4)基的介电层厚度的变化。
正如在图1和2中看到的,在与基材接触的介电层厚度相同(例如,20nm)的情况下,对于曲线C2、C3、C12和C13当叠层在与基材接触的氮化硅基的介电层和在银Ag基的功能层下面的氧化锌ZnO基的润湿层之间包含SnZnOx:Sb基的平滑层时,叠层的薄层电阻总是较低—因而较好,和对于平滑层厚度等于20nm(曲线C3和C13)的情况下,叠层的薄层电阻总是较低。
业已证实,由混合氧化物制成的平滑层在整个厚度上都是无定形的,而润湿层和金属功能层在各自的整个厚度上都是结晶的。
因此,平滑层的存在,在下层介电层厚度可比的情况下,能显著改善叠层的薄层电阻,且此种改善,当平滑层厚度大时,甚至更大。
在图3和4中,曲线分别示出,当叠层被提供有介于基材与SnZnOx:Sb基层之间的20nm氮化硅Si3N4基层时,分别在热处理之前(BHT)和之后(AHT),叠层的薄层电阻(Ω)随基于以锑掺杂的锌和锡氧化物(e SnZnOx:Sb)的平滑层厚度的变化。
还证实,由混合氧化物制成的平滑层在其整个厚度上都是无定形的,而润湿层和金属功能层则在各自整个厚度上都是结晶的。
正如还可从图3和4看出的,平滑层的存在显著改善了平滑层厚度介于>0与4nm之间的叠层的薄层电阻,且此种改善,当平滑层厚度大时,更大。
类似的结论可以适用于被提供有下阻隔涂层但没有上阻隔涂层的或者被提供有下阻隔涂层且被提供有上阻隔涂层的单功能层的叠层。
做了另一个系列的试验。
根据图5所示的单功能层的叠层结构进行3个实施例,编号为2、3和4,其中功能层40被提供有上阻隔涂层45。
下表1给出每个层的以纳米表示的厚度:
表1
层 | 材料 | 实施例2 | 实施例3 | 实施例4 |
64 | Si3N4 | 40 | 40 | 40 |
62 | ZnO | 10 | 10 | 10 |
45 | Ti | 2 | 2 | 2 |
40 | Ag | 10 | 10 | 10 |
30 | ZnO | 10 | 10 | 10 |
26 | SnZnOx:Sb | - | - | 10 |
24 | Si3N4 | 30 | 30 | 20 |
这些实施例的电阻率、光学和能量特性在下表2中给出:
表2
实施例 | R□(Ω) | RL(%) | TL(%) | a*(D65) | b*(D65) | E(%) |
2BHT | 5.7 | 4.4 | 86.5 | 2.3 | -5.2 | 6 |
2AHT | - | - | - | - | - | - |
3BHT | 6.9 | 4.4 | 85.6 | 2.9 | -7.8 | 8 |
3AHT | 5.2 | 4.5 | 87.1 | 6.5 | -6 | 6 |
4BHT | 5.8 | 5.7 | 87 | 1.3 | -3.5 | 6 |
4AHT | 4.3 | 4.3 | 88.7 | 3.3 | -5.7 | 5 |
于是,本发明实施例4在热处理之前和之后的电阻率都分别低于对比例3和2。
再有,在光源D65下测定的光反射RL(D65),透光率TL以及在LAB色度系统中在光源D65下测定的在这些层的一侧的反射时的颜色a*和b*值,在本发明实施例与对比例3和2之间没有非常显著的变化。
通过比较热处理之前与热处理之后的光学和能量特征,没有观察到重要的退化。
根据图6所示的单功能层的叠层的结构实施了其他试验,其中功能层40被提供有上阻隔涂层45但没有下阻隔涂层35。
根据图7所示的单功能层的叠层的结构实施了其他试验,其中功能层40被提供有下阻隔涂层35并且被提供有上阻隔涂层45。
所有这些试验可以得到类似的结果。
为了可以测量各层的粗糙度,另外进行了试验。
下表3给出由X-射线反射测定法测定的并以纳米为单位表示的粗糙度(基材的粗糙度为约0.4):
表3
层 | 层的厚度(nm) | 粗糙度σ(nm) |
Si3N4玻璃 | 28.5基材 | 1.1 |
SnInOx玻璃 | 29.5基材 | 0.8 |
SnZnOx:Sb玻璃 | 32.0基材 | 0.7 |
SnZnOx:SbSi3N4玻璃 | 11.219.7基材 | 0.80.5 |
SnInOxSi3N4玻璃 | 10.419.3基材 | 0.80.5 |
正如从该表可以看出的,基于唯一地沉积在玻璃上的氮化硅Si3N4的层的粗糙度虽高,但包含基于铟和锡氧化物SnInOx(ITO)的层的或者基于沉积在氮化硅基的层上的混合锌和锡氧化物SnZnOx:Sb的层的叠层最终粗糙度却较低。因此,基于混合氧化物的润湿层可以通过降低其粗糙度来改善与润湿层接触的界面的粗糙度。
上面通过实施例描述了本发明。但要知道,本领域技术人员能够进行本发明不同的方案,而不偏离如权利要求定义的本发明范围。
Claims (11)
1.基材(10),尤其是透明玻璃基材,其被提供有薄层叠层,该叠层包含具有在红外和/或日光范围反射性能的功能层(40),尤其是基于银或含银金属合金的金属功能层,以及2个涂层(20、60),所述涂层包括多个介电层(24、26;64),使得功能层(40)位于这2个涂层(20、60)之间,功能层(40)被沉积在润湿层(30)上,润湿层本身被直接沉积到下层涂层(20)上,特征在于,下层涂层(20)包含至少一个氮化物基的,尤其是氮化硅基的和或氮化铝基的介电层(24),和至少一个由混合氧化物制成的非结晶的平滑层(26),所述平滑层(26)与所述上层润湿层(30)接触。
2.权利要求1的基材(10),其特征在于,平滑层(26)是基于下列金属中的一种或多种的氧化物的混合氧化物层:Sn、Si、Ti、Zr、Hf、Zn、Ga、In。
3.以上权利要求的基材(10),其特征在于,平滑层(26)是在低温沉积的基于锌和锡并任选被掺杂的混合氧化物层或铟锡混合氧化物(ITO)的层。
4.以上权利要求中任何一项的基材(10),其特征在于,平滑层(26)是具有非化学计量的氧的氧化物层。
5.以上权利要求中任何一项的基材(10),其特征在于,平滑层(26)具有0.1~30nm,优选0.2~10nm之间的几何厚度。
6.以上权利要求中任何一项的基材(10),其特征在于,功能层(40)被直接置于至少一个下层阻隔涂层(35)上面和/或直接在至少一个上层阻隔层(45)下面。
7.以上权利要求的基材(10),其特征在于,至少一个阻隔涂层(35、45)是基于Ni或Ti的或基于镍基合金,尤其是基于NiCr合金。
8.以上权利要求中任何一项的基材(10),其特征在于,在功能层(40)下层的润湿层(30)是基于氧化锌。
9.包括至少一个以上权利要求中任何一项的基材(10)的玻璃板,任选地与至少一个其他基材结合。
10.以上权利要求的玻璃板,其以单块形式或以双层玻璃或层压玻璃型的多层玻璃形式安装特征在于,至少载有该叠层的基材被弯曲或被钢化。
11.用于制造权利要求1~8中任何一项的基材(10)的方法,其特征在于,采用任选地磁场辅助的阴极喷镀类真空技术在基材上沉积薄膜叠层,随后特征在于对所述基材实施弯曲、钢化或退火类型热处理,而不会损害其光学和/或力学品质。
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- 2006-03-06 FR FR0650771A patent/FR2898123B1/fr active Active
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2007
- 2007-03-06 BR BRPI0708389-0A patent/BRPI0708389B1/pt active IP Right Grant
- 2007-03-06 PT PT07731699T patent/PT1993965T/pt unknown
- 2007-03-06 JP JP2008557807A patent/JP5129759B2/ja not_active Expired - Fee Related
- 2007-03-06 US US12/281,480 patent/US9919497B2/en active Active
- 2007-03-06 CA CA2644888A patent/CA2644888C/fr active Active
- 2007-03-06 MX MX2008011390A patent/MX2008011390A/es active IP Right Grant
- 2007-03-06 ES ES07731699.0T patent/ES2683020T3/es active Active
- 2007-03-06 PL PL07731699T patent/PL1993965T3/pl unknown
- 2007-03-06 TR TR2018/10727T patent/TR201810727T4/tr unknown
- 2007-03-06 EA EA200870318A patent/EA017695B1/ru not_active IP Right Cessation
- 2007-03-06 KR KR1020087020748A patent/KR101400417B1/ko active IP Right Grant
- 2007-03-06 DK DK07731699.0T patent/DK1993965T3/en active
- 2007-03-06 EP EP07731699.0A patent/EP1993965B1/fr active Active
- 2007-03-06 CN CN200780008049.XA patent/CN101395096B/zh active Active
- 2007-03-06 WO PCT/FR2007/050882 patent/WO2007101964A1/fr active Application Filing
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- 2018-01-17 US US15/873,098 patent/US20180141314A1/en not_active Abandoned
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CN104025704A (zh) * | 2012-01-10 | 2014-09-03 | 法国圣戈班玻璃厂 | 带有导电涂层的透明玻璃 |
CN104025704B (zh) * | 2012-01-10 | 2016-10-12 | 法国圣戈班玻璃厂 | 带有导电涂层的透明玻璃 |
CN104884404A (zh) * | 2012-12-28 | 2015-09-02 | 日本板硝子株式会社 | 减压多层玻璃面板 |
CN104884404B (zh) * | 2012-12-28 | 2018-07-27 | 日本板硝子株式会社 | 减压多层玻璃面板 |
CN105683117A (zh) * | 2013-11-08 | 2016-06-15 | 法国圣戈班玻璃厂 | 具有改进的机械性质的涂覆有功能层叠层的基底 |
CN105683117B (zh) * | 2013-11-08 | 2020-05-19 | 法国圣戈班玻璃厂 | 具有改进的机械性质的涂覆有功能层叠层的基底 |
CN107074636A (zh) * | 2014-09-30 | 2017-08-18 | 法国圣戈班玻璃厂 | 被提供有具有热性质和亚化学计量中间层的堆叠体的基材 |
CN109790067A (zh) * | 2016-09-26 | 2019-05-21 | 法国圣戈班玻璃厂 | 用低辐射率涂层涂覆的基材 |
Also Published As
Publication number | Publication date |
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KR20080101935A (ko) | 2008-11-21 |
PL1993965T3 (pl) | 2018-10-31 |
CN101395096B (zh) | 2014-07-23 |
FR2898123B1 (fr) | 2008-12-05 |
EP1993965A1 (fr) | 2008-11-26 |
EA200870318A1 (ru) | 2009-02-27 |
FR2898123A1 (fr) | 2007-09-07 |
US20180141314A1 (en) | 2018-05-24 |
JP2009528932A (ja) | 2009-08-13 |
BRPI0708389B1 (pt) | 2017-12-26 |
EP1993965B1 (fr) | 2018-05-16 |
KR101400417B1 (ko) | 2014-05-26 |
DK1993965T3 (en) | 2018-08-27 |
JP5129759B2 (ja) | 2013-01-30 |
BRPI0708389A2 (pt) | 2011-05-24 |
US9919497B2 (en) | 2018-03-20 |
CA2644888C (fr) | 2015-06-16 |
WO2007101964A1 (fr) | 2007-09-13 |
US20090197077A1 (en) | 2009-08-06 |
MX2008011390A (es) | 2008-09-18 |
PT1993965T (pt) | 2018-10-10 |
CA2644888A1 (fr) | 2007-09-13 |
TR201810727T4 (tr) | 2018-08-27 |
EA017695B1 (ru) | 2013-02-28 |
ES2683020T3 (es) | 2018-09-24 |
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