CN107112672A - 装配有导电装置并具有改善的耐温度循环测试性的窗玻璃 - Google Patents
装配有导电装置并具有改善的耐温度循环测试性的窗玻璃 Download PDFInfo
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Abstract
本发明涉及一种由至少一个基材构成的窗玻璃,该基材的一部分包含导电元件,所述导电元件包含由含铬钢制成的连接器,该连接器用基于锡、银和铜的焊料合金焊接到导电轨道上,其中通过包含银粉末和玻璃料的混合物的银糊料的烧结形成的导电轨道具有低于或等于3.5μΩ·cm的在25℃下测量的电阻率和低于20%的孔隙度水平,所述孔隙度水平通过扫描电子显微镜在包含导电轨道并已经通过离子研磨进行预先抛光的基材部分的横截面上进行测量。
Description
本发明涉及包含电连接元件的窗玻璃,其制备方法及其在用于交通工具的窗玻璃的领域中的用途。
本发明更特别地涉及具有电功能的汽车用窗玻璃,如,例如加热或除霜的窗玻璃或者配备有天线的窗玻璃。存在于汽车用窗玻璃中的加热丝、天线或其它传感器是由导电糊料(如例如丝网印刷到玻璃基材上的含银糊料)形成的导电轨道,并通过焊接到导电糊料的连接器连接到电源。由于在这些系统中使用的材料的热膨胀系数不同,在这些窗玻璃的制备和处理期间出现机械应变或应力,在该窗玻璃中引起脆化并出现裂纹,特别是在这些连接器的定位处。目前使用的焊料合金通常是基于铅,因此基于高延展性的金属。这允许通过由制备商指定的电阻测试而不出现裂纹,裂纹使得窗玻璃不合适用于期望的用途。欧洲指令目前禁止使用这种铅基合金,并且已经进行了许多工作,以寻找能够替代铅基合金的其它焊料合金。使用含锡、银和铜的合金可获得良好的折中。这些合金同时具有允许其焊接的优良性能和通过汽车制备商目前规定的测试所需的坚固性。与从焊料合金中除去铅的这个潜在问题并行地,对所述连接器进行的老化测试变得更加严格;特别是对温度循环测试的条件变得更加严格。这些测试以英文术语“Temperature Cycling Test”或TCT所已知。这些测试的目的是确定窗玻璃是否能够承受连续快速的温度升高和降低,而不会变得脆化。这些测试已经被开发用于加速由于系统的不同组件的热行为的差异而引起的影响。新测试规定温度在-40℃和+105℃之间变化,因此该变化范围比以前测试的变化范围(其限制在90℃)更大。循环次数也已经被改变,因为它从10个循环到最少60个循环。新的TCT条件还要求在温度升高阶段期间这些温度变化在14V的电压下进行实施,从而产生附加热量并对应于可高达约120℃的局部温度。尽管对连接器的形状和材料的选择进行优化,目前已知和使用的系统不是足够耐用的,并且在更严格的测试之后会出现裂缝或裂纹。事实上,与铅基合金相比,基于锡、银和铜的合金更大的刚度导致更多的应力被转移直至基材。与更严格的TCT测试相结合的这种合金的物理性能导致在窗玻璃中产生更多的缺陷或裂纹。达到的更高温度还导致连接器和焊料合金的更大的热膨胀,其引起电连接元件其整体上更大的应力。因此,配备这种类型的连接器和合金的窗玻璃不符合这些测试规定的标准,因此变得不符合由制备商规定的标准。
本发明涉及一种由基材构成的窗玻璃,该基材包含被沉积在基材上的电连接系统,该电连接系统由至少一个电连接器、导电金属糊料和焊料合金组成,所述系统面对温度行为测试时具有更好的耐用性,这是由于它允许在温度升高和降低的测试后在基材中可能出现的裂纹的数量显着降低。
本发明的一个目的是一种由基材构成的窗玻璃,所述基材的至少一部分包含导电元件,所述导电元件包含由含铬钢制成的连接器,该连接器用基于锡、银和铜的合金焊接到导电轨道上,其中基于银的导电轨道具有低于或等于3.5μΩ·cm的在25℃时测量的电阻率和低于20%的孔隙度水平,所述孔隙度水平为通过扫描电子显微镜从包含导电轨道并且已通过离子抛光进行预先抛光的基材部分的横截面上进行测量。根据本发明的窗玻璃是一种耐受规定60个连续的循环的TCT测试的窗玻璃,在所述循环期间,使温度在-40℃和+105℃之间变化,其中在温度升高阶段期间,在14V的电压下进行。
令人惊奇地,发明人已经发现通过选择用于连接器的特定材料,特定的焊料合金类型和同时具有低孔隙度水平和低的特定电阻率的含银导电糊料,可以获得能够经受新TCT测试条件的用于汽车窗玻璃的电连接系统。
在讨论导电性糊料的焙烧时,是指在550-700℃的温度下持续2-10分钟的时间段的在空气下的热处理,其允许将导电银糊料固定在基材上。允许表征导电糊料的测量在其焙烧之后进行。
银基导电轨道是包含银粉和玻璃料的混合物的烧结银糊料。有利地,银糊料包含一些具有不同尺寸的颗粒,其中存在尺寸小于500nm的小颗粒。优选地,小颗粒为其直径为低于500nm的球形。在烧结和离子研磨之后,通过扫描电子显微镜观察该涂覆有银导电轨道的基材的横截面获得的图像上测量银粒子的尺寸和形状。
有利地,存在于导电轨道中的银颗粒的粒度使得平均直径D10小于1.1μm,直径D10表示其中10%的颗粒具有低于该值的直径。优选地,直径D10小于0.8μm。粒度测量用激光粒度计,例如Mastersizer MS2000进行。
通过丝网印刷在基材的至少一部分上沉积的银糊料层的显微分析(microanalyse)来确定银导电轨道的孔隙度水平。使用扫描电子显微镜的观察对涂覆有所述导电轨道的基材部分的横截面进行实施。通过扫描电子显微镜(MEB)获得的图像显示了对应于银糊料的浅灰色区域,对应于在导电糊料中存在的玻璃料的更深灰色区域,和表示该层的孔隙的黑色区域。该层的孔隙度水平通过给定区域的图像的处理来确定黑色区域的百分比进行计算。例如,在基材的横截面的50μm的长度上进行观察,图像通过MEB以5000的放大倍数和使用10kV的电压来获得。孔隙度水平以百分比表示,并且是对应于在观察10个不同位置之后获得的孔隙度水平的不同值的平均值的值。
因此,用于测量在本发明中使用的导电轨道的孔隙度水平的方法为如下:
1)使用电子显微镜观察用所述轨道涂覆的基材部分的横截面的约50μm的长度,该横截面通过离子研磨进行抛光;
2)通过图像处理确定所观察到的并指示孔隙的黑色区域的量,以确定以黑色区域相对于所观察表面整体的百分比表示的孔隙度水平;
3)对抛光的横截面的至少十个不同区域重复步骤1和2,以获得至少十个孔隙度水平的值;
4)计算获得的孔隙度水平值的平均值。
对于限制裂缝的传播关键的是,导电轨道是“较少孔隙的”,即其孔隙度水平低于20%。
优选地,银基导电轨道具有的孔隙度分布使得90%的孔的最大长度低于6μm。孔隙尺寸通过扫描电子显微镜在包含导电轨道的基材部分的横截面(在焙烧之后并已通过离子研磨进行预先抛光)上进行测量。
除了这种与层的孔隙度水平有关的条件之外,还需要的是,银导电轨道具有低于或等于3.5μΩ.cm的电阻率,该电阻率在25℃的温度下进行测量。小于3.5μΩ·cm的电阻率允许确保银导电糊料和由铬基钢制成的焊料合金之间良好的相容性。以欧姆·厘米表示的电阻率ρ通过测量由银导电线的电阻R(以欧姆为单位)并考虑到长度l(以m为单位)和导电线S的横截面积(以m2为单位)。
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导电线的横截面的测量例如使用接触或非接触的轮廓测量法进行实施。电阻率的测量通常对1米长的导线(méandre)进行实施。
用于丝网印刷所述导电轨道的导电银糊料有利地包含90至97重量%的银,其余为玻璃料。这种银含量对应于在导电糊料的焙烧后的含量。在焙烧后测量的银导电轨道的厚度为2μm至30μm,优选5至15μm。
用于将电连接器焊接到银导电轨道的合金是基于锡、银和铜的合金。它为一种被认为是“无铅”的合金,符合由欧洲指令所规定的标准。用于将连接器焊接到根据本发明的窗玻璃的合金是这样一种合金,其包含90至99.5重量%的锡,优选为93至99重量%的锡,更优选为95至98重量%的锡。除锡之外,它还包含0.5至5重量%的银和0至5重量%的铜。该合金还可以含有铋、铟、锌和/或锰。非常优选地,焊料合金是包含96.5重量%的锡,3重量%的银和0.5重量%的铜的合金。使焊料合金设置在电连接器的下部上。焊料合金层的厚度优选低于或等于600μm,并进一步优选为150-600μm。
电连接器由含铬钢制成。非常优选地,电连接器由不锈钢制成,即由包含至少10.5重量%铬的钢制成。这种类型的连接器具有与基于锡、铜和银的焊料合金相容的优点。事实上,不同材料必须具有允许它们结合使用的热膨胀系数,而没有产生过高的机械应力的风险,过高的机械应力将引起脆弱区和裂纹的传播。由不锈钢制成的连接器的导热率为约25-30W/mK,这高于例如由钛基合金制成的连接器的导热率。这种更高的导热率有利于焊接过程,这是由于更均匀的加热。例如,不锈钢连接器具有比铜基连接器膨胀更小的优点。特别合适的不锈钢合金是例如根据标准EN 10 088-3的钢1.4016、1.4113、1.4509和1.4510。连接器优选具有为0.1-2mm,更优选为0.2-1mm,进一步优选为0.3-0.8mm的厚度。
连接器在与焊料合金接触的表面上任选地具有基于镍、铜、锌、锡、银、金或它们的合金的润湿层或润湿涂层。优选地,这种涂层基于镍和/或银。这种涂层的厚度对于镍优选为0.1μm至0.3μm,对于银为3至20μm。
根据一个实施方式,电连接器在其旨在被设置在基材上的下表面上具有至少两个接点(plots)或至少一个垫片,其使得可以确保在连接器和银导电层之间的连接由焊料合金恰当地实现。这些接点或垫片使得该系统更坚固,这是因为有助于容纳合金并防止具有含不均匀量的焊料合金的区域,这种区域可能导致在不同构件之间具有较差粘附的区域。这些接点或垫片还允许减小可以在连接器元件和基材之间存在的机械应力。它们有利地具有圆形形状,并且特别地在专利申请US2014/0110166中进行描述。这些接点或垫片优选具有0.5×10-4m至10×10-4m的宽度和0.5×10-4m至5×10-4m的高度。这些接点或垫片的存在特别地允许控制位于连接器下方的焊料合金的厚度。事实上,有利的是使合金的厚度保持尽可能地均匀以避免任何堆积物,该堆积物可产生特定脆弱区,因为应变随着厚度的增大而变得更大。
连接器还可以被提供有至少一个接触凸块,其允许更容易焊接连接器。该接触凸块位于该连接器的待焊接区域上。
在其上放置有电连接系统的基材优选地由玻璃制成,更特别地由平板玻璃(其例如使用漂浮方法进行制备)制成,在漂浮方法中将熔融玻璃倒在熔融金属浴上。它可以例如是石英玻璃,硼硅酸盐玻璃,铝硅酸盐玻璃和/或钠钙玻璃。该基材也可以是聚合物类型,并且可以包含聚乙烯、聚丙烯、聚碳酸酯、聚甲基丙烯酸甲酯、聚苯乙烯、聚丁二烯、聚腈、聚酯、聚氨酯、聚氯乙烯、聚丙烯酸酯、聚酰胺、聚对苯二甲酸乙二醇酯和/或它们的共聚物或它们的共混物。基材优选是透明的。它具有为0.5mm至25mm,优选为0.5至10mm的厚度。
基材可以是淬火玻璃或非淬火玻璃。通过使用淬火玻璃,使表面层增强,其因此变得更坚实的,这允许更容易证实由于电连接系统的存在所产生的脆弱化现象。
本发明还涉及一种用于制备由至少一个具有电连接系统的基材构成的窗玻璃的方法,所述方法包括以下步骤:
a)将基于锡、铜和银的焊料合金施加到由铬基钢制成的电连接器的至少一个接触区域上;
b)将具有焊料合金的电连接器放置在银导电轨道上,该银导电轨道被沉积在裸露的或具有涂层的基材上,所述轨道具有低于或等于3.5μΩ.cm的在25℃测量的电阻率和低于20%的孔隙度水平,所述孔隙度水平通过扫描电子显微镜在包含该电连接系统的基材部分的通过离子研磨进行抛光的横截面上进行测量;和
c)将连接器的接触区焊接到银导电轨道。
优选地,在步骤a)期间,在连接器的接触区上沉积少量的呈片或扁平滴形式的焊料合金。沉积合金的形状,体积和厚度是预先确定的。优选地,沉积的焊料合金片的厚度小于或等于0.6mm。其形状优选地与接触区域的形状相同,以确保后者在其整个表面上与导电轨道接触。
银导电轨道通过使用本领域技术人员已知的方法,例如通过丝网印刷,在基材上沉积导电银糊料(银基搪瓷)来获得。导电银糊料层的沉积是独立于步骤a)进行实施的,只要它可以在步骤a)之前,期间或之后进行。银糊料层可以直接被沉积在基材上,或者沉积在层(该层本身被沉积在基材上)上。因此,导电银糊料层可以被沉积在黑色搪瓷层上,该黑色搪瓷层被沉积在基材上并且主要旨在使得从窗玻璃的外部看不到电连接系统。
一旦被沉积,导电糊料层随后在约150℃进行干燥,然后在空气中在550℃至700℃之间的温度下焙烧2到10分钟的时间段(烧结步骤)。如此烧结的银基搪瓷是固体形式。接触端子或连接器可以被焊接以允许导电线被供电。
连接器在银导电轨道上的焊接可以通过冲压、活塞焊接、微火焰焊接、激光焊接、热空气焊接、感应焊接、电阻焊接和/或使用超声波来实现。
本发明还涉及包含至少一个如上所述的电连接系统的窗玻璃在建筑物或交通工具中,特别是汽车交通工具,轨道交通工具或飞机中的用途。窗玻璃特别地用作为加热式的或配有天线或配有被设置在窗玻璃中或在窗玻璃上的任何其它电功能的挡风玻璃、侧窗、后挡风玻璃或车顶。
以下实施例非限制性地举例说明本发明。
温度升高和降低测试或“温度循环测试”是在标准EN ISO 16750-4-H第5.3.1.2节
中描述的测试。所述循环的温度和持续时间如在下表中所示:
持续时间(min) | 温度(℃) |
0. | +20 |
60 | -40 |
150 | -40 |
210 | 20 |
300 | +105 |
420 | -105 |
480 | +20 |
在这些循环中,在测量室中的湿度不进行控制。样品经历至少60个连续循环。在温度升高的阶段(标准VW80101)中对样品施加14V(+/-0.2)的电压。
图1是通过扫描电子显微镜观察到的不符合本发明的样品的图像,在该图像中观察到导电层(1)的高孔隙度水平(高于20%)。
图2和图3是通过扫描电子显微镜观察到的根据本发明的样品的图像,在该图像中观察到导电层(1)的低孔隙度水平(低于20%)。
在这些照片中,浅灰色区域(2)对应于银导电层(1),更深灰色区域(3)对应于玻璃料和黑色区域(4)对应于银层的孔隙。
在这些图中,导电层(1)被沉积在搪瓷层(5)上。
在以下实施例中,在将银糊料分散在丙酮中之后,粒度的测量使用MastersizerMS2000激光粒度计进行实施,该粒度计使用He-Ne激光型红光源和LED型蓝光源进行操作。为了制备样品,将50mg银糊料稀释在20mL丙酮中。
孔隙尺寸的测量,特别是其最大长度的测量由在导电糊料焙烧后通过扫描电子显微镜观察到的图像进行实施。
比较实施例1(不符合本发明)
多个样品通过在玻璃基材的区域(在该区域中已沉积了黑色搪瓷层)上沉积导电银糊料层进行制备。这种糊料的银颗粒基本上呈其尺寸为0.5-10μm的薄片形式。银颗粒的粒度使得平均直径D10为1.25μm。银糊料层和搪瓷层通过丝网印刷,使用编织为77.55目的筛网形式的聚酯线织物进行沉积。使银糊料在150℃进行干燥,然后在空气中在640℃的温度烧结140秒,然后将如此涂覆的基材进行淬火。将如此获得的样品进行切割并放置在离子磨机中以抛光其横截面。该抛光在2小时的抛光周期中用Hitachi IM4000型抛光机进行实施,该抛光机在氩气流下进行使用6kV的电压进行运行。然后在扫描电子显微镜中通过检测反向散射电子(使用5000的放大倍数、在10kV的电压下)进行观察。该观察在长度为50μm的区域上进行实施。孔隙度水平通过测量在所研究样品中的黑色区域的百分比进行评估。通过使用软件Image Pro来分析获得的图像。由此获得的导电轨道具有约30%的通过扫描电子显微镜测量的孔隙度水平。孔隙的最大长度L90为8.5μm。
电阻率的测量使用Taylor Hobson Talysurf 50牌表面轮廓仪进行实施,以确定1米长的导线的横截面。导电轨道的电阻率在25℃时为4.5μΩ.cm。
将不锈钢连接器(参考编号1.4016)使用Sn96.5Ag3Cu0.5合金通过感应焊接到银导电轨道上。在该焊接步骤之前,将窗玻璃基材已预热至60℃,并且导电轨道已经受使用钢丝绒刷的表面刷涂。
然后使在其上焊接有电连接器的玻璃基材经受连续60次的上述的温度循环。
在这些测试之后,在所有制备的样品中观察到明显的裂纹。因此,这些样品不符合由温度变化测试所要求的标准。
根据本发明的实施例2
以与在实施例1中所描述的操作方式相同的操作方式,使用不同的导电银糊料制备了样品。使用的搪瓷与实施例1相同。这种糊料的银颗粒基本上呈其尺寸为1μm至6μm的片形式和尺寸为140-400nm的球形颗粒形式。银颗粒的粒度使得平均直径D10为0.46μm。由这种银糊料获得的导电轨道在25℃时具有16%的孔隙度水平和为3.2μΩ.cm的电阻率。孔隙的最大长度为3.5μm。所使用的焊料合金和连接器也与实施例1相同。对不同样品进行了两种类型的焊接(感应焊接和电阻焊接)。然后使样品在与在实施例1中所述条件相同的条件下经受了温度变化循环测试。
所有样品均成功通过测试,没有出现裂缝。
根据本发明的实施例3
以与在实施例1中所描述的操作方式相同的操作方式,使用与实施例1和2不同的导电银糊料制备样品。使用的搪瓷与实施例1相同。这种糊料的银颗粒基本上呈其尺寸在1.2至2.4μm之间的球体形式和其尺寸在70至400μm之间的更小颗粒形式。银颗粒的粒度使得平均直径D10为0.43μm。从这种银糊料获得的导电轨道具有为15%的孔隙度水平和在25℃时为2.8μΩ·cm的电阻率。孔隙的最大长度为1.8μm。所使用的焊料合金和连接器也与实施例1相同。对不同样品测试了两种类型的焊接(感应焊接和电阻焊接)。然后使样品在与实施例1所述的条件相同的条件下经受温度变化循环测试。
所有样品均成功通过测试,没有出现裂缝。
根据本发明的实施例4
使用与实施例2中所使用的黑色搪瓷不同的黑色搪瓷制备与实施例2中所描述的样品相同的样品。所述系统的其它构件与实施例2中所述的相同。如此得到的所有样品均成功通过了测试,没有出现裂纹。
Claims (19)
1.一种由基材构成的窗玻璃,其至少一部分包含导电元件,所述导电元件包含由含铬钢制成的连接器,该连接器用基于锡、银和铜的焊料合金焊接到导电轨道上,其中基于银的导电轨道具有低于或等于3.5μΩ·cm的在25℃下测量的电阻率和低于20%的孔隙度水平,所述孔隙度水平通过扫描电子显微镜在包含导电轨道并已经通过离子研磨进行预先抛光的基材部分的横截面上进行测量。
2.根据前述权利要求所述的窗玻璃,其特征在于,导电轨道是包含银粉和玻璃料的混合物的烧结银糊料。
3.根据前述权利要求中任一项所述的窗玻璃,其特征在于,所述基于银糊料的导电轨道具有孔隙度分布,使得90%的孔隙的最大长度低于6μm。
4.根据前述权利要求中任一项所述的窗玻璃,其特征在于,所述银糊料包含具有不同尺寸的颗粒,其中存在尺寸小于500nm的小颗粒。
5.根据权利要求4所述的窗玻璃,其特征在于,所述小颗粒具有直径小于500nm的球形状。
6.根据前述权利要求中任一项所述的窗玻璃,其特征在于,存在于导电轨道中的银颗粒的粒度使得平均直径D10小于1.1μm,其中直径D10表示这样的直径,其中10%颗粒的直径小于这种直径值。
7.根据前述权利要求中任一项所述的窗玻璃,其特征在于,所述焊料合金是包含90至99.5重量%的锡,优选93至99重量%的锡,更优选95至98重量%锡的合金。
8.根据权利要求7所述的窗玻璃,其特征在于,除锡之外,焊料合金还包含0.5至5重量%的银和0至5重量%的铜。
9.根据前述权利要求中任一项所述的窗玻璃,其特征在于,所述焊料合金是包含96.5重量%的锡,3重量%的银和0.5重量%的铜的合金。
10.根据前述权利要求中任一项所述的窗玻璃,其特征在于,所述电连接器由不锈钢制成。
11.根据前述权利要求中任一项所述的窗玻璃,其特征在于,所述电连接器在其旨在被设置在所述基材上的下表面上具有至少两个接点或垫片。
12.根据前述权利要求中任一项所述的窗玻璃,其特征在于,在烧结后测量的银导电轨道的厚度为2至30μm,优选地为5至15μm。
13.根据权利要求中任一项所述的窗玻璃,其特征在于,所述基材是淬火玻璃。
14.根据权利要求1至12中任一项所述的窗玻璃,其特征在于,所述基材是非淬火玻璃。
15.一种用于制备由至少一个具有电连接系统的基材构成的窗玻璃的方法,所述方法包括以下步骤:
-将基于锡、铜和银的焊料合金施加到由铬基钢制成的电连接器的至少一个接触区域上;
-将被提供有焊料合金的电连接器放置在银导电轨道上,该银导电轨道被沉积在裸露的或具有涂层的基材上,所述轨道具有低于或等于3.5μΩ.cm的在25℃测量的电阻率和低于20%的孔隙度水平,所述孔隙度水平通过扫描电子显微镜在包含导电轨道的并通过离子研磨进行抛光的基材部分的横截面上进行测量;和
-将连接器的接触区焊接到银导电轨道。
16.根据前一项权利要求所述的方法,其特征在于,在步骤a)期间,在所述连接器的接触区域上沉积厚度小于或等于0.6mm的薄片或扁平滴。
17.根据权利要求15和16中任一项所述的方法,其特征在于,所述连接器在银导电轨道上的焊接通过冲压、活塞焊接、微焰焊接、激光焊接、热空气焊接、感应焊接、电阻焊接、烙铁焊接和/或超声波焊接进行实施。
18.根据权利要求1至14中任一项所述的窗玻璃在建筑物或交通工具中,特别地在汽车交通工具,轨道交通工具或飞机中的用途。
19.根据权利要求18所述的用途,其用作为加热式的或配有天线或配有被设置在窗玻璃中或在窗玻璃上的任何其它电功能的挡风玻璃、侧窗、后挡风玻璃或车顶。
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FR1562116A FR3044962B1 (fr) | 2015-12-10 | 2015-12-10 | Vitrage muni d'un dispositif conducteur electrique et possedant une resistance amelioree aux tests cycliques de temperature. |
FR1562116 | 2015-12-10 | ||
PCT/FR2016/053274 WO2017098164A1 (fr) | 2015-12-10 | 2016-12-08 | Vitrage muni d'un dispositif conducteur electrique et possedant une resistance amelioree aux tests cycliques de temperature |
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WO2011010659A1 (ja) * | 2009-07-21 | 2011-01-27 | 日亜化学工業株式会社 | 導電性材料の製造方法、その方法により得られた導電性材料、その導電性材料を含む電子機器、および発光装置 |
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EP2024428B1 (en) * | 2006-06-02 | 2010-12-01 | Exatec, LLC. | Photochromatic effect for polycarbonate glazing applications |
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US20180368268A1 (en) | 2018-12-20 |
KR20180091879A (ko) | 2018-08-16 |
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RU2018121047A (ru) | 2020-01-10 |
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BR112018006137A2 (pt) | 2018-10-23 |
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BR112018006137B1 (pt) | 2022-03-03 |
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DK3386747T3 (da) | 2022-08-01 |
KR102662932B1 (ko) | 2024-05-07 |
EP3386747A1 (fr) | 2018-10-17 |
CA2999950A1 (fr) | 2017-06-15 |
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US10512169B2 (en) | 2019-12-17 |
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