CN102639455A - 电致变色器件 - Google Patents

电致变色器件 Download PDF

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CN102639455A
CN102639455A CN2010800422573A CN201080042257A CN102639455A CN 102639455 A CN102639455 A CN 102639455A CN 2010800422573 A CN2010800422573 A CN 2010800422573A CN 201080042257 A CN201080042257 A CN 201080042257A CN 102639455 A CN102639455 A CN 102639455A
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J-C.吉龙
R.吉
T.贝尔坦-穆罗
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Saint Gobain Sekurit Deutschland GmbH
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Abstract

本发明涉及包括其线性热膨胀系数为35-60×10-7/℃的第一非淬火玻璃基材(S1)的电致变色器件，所述基材(S1)被包括至少一个透明导电层(2、4)、电致变色材料层(EC2)、离子导电电解质层(EL)和对电极(EC1)的堆叠体涂覆。所述基材的重量百分比组成为如下：SiO2 50至82；B2O3 0至20；Al2O30至22；MgO 0至10；CaO 0至15；SrO 0至5；BaO 0至15；CaO+MgO+BaO+SrO 0至15；Na2O 0至6；K2O 0至8；Na2O+K2O 0至8。

Description

电致变色器件
本发明涉及具有受控透明度的电致变色器件，尤其用于构成电控窗玻璃的的电致变色器件，及其制造方法。其还涉及配有这种器件的电致变色窗玻璃以及该器件用于最广泛应用的用途。
其透光能力可从良好的透明水平调节直至最完全的不透明的窗玻璃是已知的。这种窗玻璃已显示可用于最广泛的技术领域。
它们因此可用作住宅窗玻璃，以便例如它们可根据室外条件和随用户的希望调节进入住所的日照水平。它们也可用作隔离百叶窗(voelts d’isolation)以保护住所的居民的隐私（对于室外或对于邻室）。
在运输交通工具领域中，此类器件可用于例如调节汽车的挡风玻璃和/或侧窗或天窗玻璃的透明度水平以及用在运输交通的某些工具配件，尤其例如后视镜上以控制反射向驾驶者的光通量并防止其被光晃眼。当然，该器件可用于其它领域，特别是在航空领域中，以例如控制飞机舷窗的透明度。
由于电致变色器件在它们的不透明状态下是吸收性的，它们暴露在光，尤其是日光中时容易被强烈加热。这特别是用作窗玻璃的电致变色器件的情况。当这些窗玻璃安装在框架中，例如当应用在建筑物幕墙中时，结果常常是出现玻璃中心与其边缘之间的热梯度，这可造成窗玻璃破裂。明亮日光中的阴影也可产生相同现象。因此，电致变色器件中所用的钠钙硅玻璃基材目前进行淬火或硬化以具有更好的热-机械强度。但是，淬火或硬化玻璃的使用也具有其缺点：这些玻璃不能切割，因此必须在具有它们最终尺寸的玻璃基材上进行薄层沉积。根据相关建筑项目，所述最终形状非常不同。当通过磁控管阴极溅射沉积薄层时，将各种尺寸的基材置于金属基材载体上。这时需要通过考虑玻璃板与基材支持体之间的表面积比逐一地调节层的沉积参数。该方法因此变得难以控制。出于经济和后勤原因和生产容易性，因此优选能在标准尺寸，通常地大尺寸的基材上沉积这些薄层，随后将基材切割成所需尺寸。
本发明人已能证实，借助于使用已明确测定其线性热膨胀系数的玻璃基材实现这一目标。
本发明的主题因此是包含其线性热膨胀系数为35-60×10-7/℃的第一非淬火玻璃基材的电致变色器件，所述基材被包含至少一个透明导电层、电致变色材料层、离子导电电解质层(couche d’un electrolyte conducteur ionique)和对电极的堆叠体涂覆。实际上，目前使用的钠钙硅类型的玻璃具有大约89×10-7/℃的热膨胀系数。
线性膨胀系数是指平均线性膨胀系数。可以在接近环境温度(通常20℃、30℃或甚至50℃)的温度下和在低于玻璃的玻璃化转变温度(例如300℃，或400℃，甚至500℃)的温度之间测量这种系数。通常，所考虑的温度范围是20℃-300℃范围。由于玻璃的伸长在低于玻璃化转变温度的温度范围内随温度线性变化，温度的选择不明显地影响结果。
本发明中的器件优选包括第二玻璃基材，常被称作正面基材。这种第二基材还可具有如定义的线性热膨胀系数，或相反，标准线性热膨胀系数，例如大约85-90×10-7/℃。
优选地，第一玻璃基材具有小于或等于50×10-7/℃，甚至小于或等于45×10-7/℃的线性热膨胀系数。
第一玻璃基材优选是二氧化硅基氧化物玻璃，在SiO2含量大于或等于40%，尤其是50%的意义上来说。在全文中，所述含量是重量含量。
第一玻璃基材优选具有包括下列氧化物的化学组成：SiO2、Al2O3和至少一种碱土金属氧化物。
除上文提到的氧化物外，基材的组成还可含有氧化硼(B2O3)和/或至少一种碱金属氧化物。
基材的组成还可含有一种或多种下列氧化物：ZrO2、P2O5、ZnO、SnO2、SO3、As2O3、Sb2O3。
该基材还可含有一种或多种着色剂，尤其提到：
- 铁、钒、钛、铬、锰、钴、镍、铜、铈、钕、镨和铒的氧化物，
- 胶体形式的金属，如铜、银或金，或元素或离子形式的那些，如硒或硫。
二氧化硅(SiO2)含量优选为50至75%，尤其是50至65%。高含量实际上伴随着粘度提高。
氧化铝(Al2O3)含量优选为1至20%，尤其是5至15%。高氧化铝含量可造成玻璃粘度提高以及反玻璃化倾向提高。
氧化硼(B2O3)可用于同时降低玻璃的粘度及其热膨胀系数。该含量优选小于或等于20%，优选15%。
碱土金属包括镁、钙、锶、钡。钙和镁由于它们的低成本和对玻璃密度的低影响而是优选的。碱土金属的氧化物可用于降低玻璃的粘度和促进熔化，而不过度损害膨胀系数。但是，在大量时，它们可引起促进玻璃反玻璃化。它们的总含量因此优选小于或等于25%，或甚至20%和甚至15%。
碱金属包括锂、钠、钾，后两种由于它们的低成本而是优选的。碱金属的氧化物具有通过降低玻璃粘度及其反玻璃化倾向而促进玻璃熔化的作用。但是，这些氧化物造成热膨胀系数显著提高，以致它们的总含量优选小于或等于8%，尤其是6%和甚至5%。
第一基材优选具有在下面规定的重量范围内包含以下成分的化学组成：
SiO2                                         50至82%，尤其50至75%
B2O3                                        0至20%
Al2O3                                       0至22%
MgO                                        0至10%
CaO                                         0至15%
SrO                                          0至 5%
BaO                                         0至15%
CaO+MgO+BaO+SrO            0至15%, 尤其5至15%
Na2O                                       0至6%
K2O                                         0至8%
Na2O+K2O                              0至8%。
更优选地，第一基材具有在下面规定的重量范围内包含以下成分的化学组成：
SiO2                                     50至60%
B2O3                                          10至15%
Al2O3                                         10至15%
MgO                                          2至5%
CaO                                           2至5%
SrO                                            0至1%
BaO                                           0至1%
CaO+MgO+BaO+SrO              5至15%
Na2O                                         0至5%
K2O                                           0至5%
Na2O+K2O                                1至6%。
所述或每个玻璃基材可以使用本领域技术人员熟悉的技术进行制造。混合通常粉末形式的原材料(天然的或来自化学工业)，随后引入炉中。通过燃烧器(架空、浸在玻璃浴中和/或位于炉顶，其作用于原材料或玻璃浴)或再通过使用浸在玻璃浴中的电极，通常钼电极加热该炉。该炉应通常由耐火砖，例如二氧化硅、氧化铝、富铝红柱石、氧化铬和/或在氧化铝-氧化锆-二氧化硅固溶体中构成。原材料在热作用下经历各种反应，引起获得熔融玻璃浴。玻璃浴的温度通常为1300至1700℃，尤其是1550至1650℃。随后将该熔融玻璃输送到成型设备中：例如通过倾倒在熔化锡浴上(该方法称为“浮法”)或通过使用层压辊来成型。通常将所得玻璃板退火以消除在冷却过程中在其中可能产生的任何机械应力。
本发明的电致变色器件优选包含，以从第一基材开始的顺序或以逆顺序：
- 透明导电层，
- 对电极，使得可以可逆***具有与该电致变色材料相同的电荷的离子，
- 离子导电电解质层，
- 电致变色材料层，使得可逆并同时***离子，在所述离子经受适当电能时，与***和去除的状态对应的所述离子氧化态为不同着色；这些状态之一具有比另一个状态更高的光透射，
- 第二透明导电层。
或者，可以颠倒这两个透明导电层之间的层顺序：
电致变色材料，随后电解质，最后对电极。
该电致变色材料优选基于氧化钨(阴极电致变色材料)或氧化铱(阳极电致变色材料)。这些材料可***阳离子，尤其是质子或锂离子。
对电极优选由中性着色层，或至少，在电致变色层为有色态时，透明或略微有色的层构成。对电极优选基于选自钨、镍、铱、铬、铁、钴、铑的元素的氧化物，或基于这些元素至少两种的混合氧化物，尤其是镍和钨的混合氧化物。如果该电致变色材料是氧化钨(因此，阴极电致变色材料，其有色态代表其最还原态)，基于氧化镍或氧化铱的阳极电致变色材料可以例如用于对电极。这特别可以是钒和钨混合氧化物层或镍和钨混合氧化物层。如果该电致变色材料是氧化铱，阴极电致变色材料(例如，基于氧化钨)可充当对电极。也可以使用为相关氧化态的光学中性材料，例如氧化铈，或有机材料，如电子导电聚合物(聚苯胺)或普鲁士蓝。
使用第一实施方案，电解质以聚合物或凝胶形式存在，尤其是质子传导聚合物(例如，如在欧洲专利EP 0 253 713和EP 0 670 346中描述的那些)或锂离子传导聚合物(例如，如在专利EP 0 382 623、EP 0 518 754或EP 0 532 408中描述那些)。其这时被称作混合电致变色***。
根据第二实施方案，电解质由形成离子导体的矿物层(其是电绝缘的)构成。这些电致变色***这时被称作“全固体”。尤其可以参考欧洲专利EP 0 867 752和EP 0 831 360。
本发明的器件也可以是“全聚合物”类型，其中两个导电层分置于包括阴极着色聚合物、离子(尤其是H+或Li+)导电电子绝缘聚合物和最后阳极着色聚合物(如聚苯胺或聚吡咯)的堆叠体的两侧。
电致变色堆叠体还可以包括各种层，尤其是例如旨在促进后继层沉积或保护某些层免受机械或化学侵袭(防腐蚀、防磨损等)的下层、上层或中间层。电致变色堆叠体可例如在上面有二氧化硅基和/或氧化铝基保护层。
本发明中的器件可以如下制造：在透明或不透明的载体基材上先后沉积下导电电极(通常为氧化铟锡(ITO)层或掺杂的氧化锡层，例如用氟掺杂），电致变色功能层（例如氧化铱(IrOx)、氧化钨(WO3)、氧化钽(Ta2O5)）和上导电电极。
当然，所述两个下和上导电电极必须连接到分别的电源接头上。通常使用分别与上和下电极接触的金属箔获得这种连接。
该电致变色器件通常包括第二基材(第一基材是在其上沉积电致变色堆叠体的基材)。几种实施方法是可行的：可以层压两个基材，在将层压聚合物(尤其基于聚乙烯醇缩丁醛，基于乙烯和乙酸乙烯酯的共聚物－EVA－，或聚氨酯)接触地放置在第一基材（被其堆叠体覆盖）与第二基材之间意义上来说。或者，这两个基材可以双层玻璃形式安装，在第二基材保持离第一基材一定距离的意义上来说，通常借助在这两个基材之间安排气体腔的四周框架。该气体尤其是氩气。在这两种情况下，都将电致变色堆叠体设置于两个基材之间以保护其不受任何类型的化学或机械侵袭。
图1示意性表示本发明的电致变色器件。
参照图1，本发明的电致变色器件优选是“全固体”并相继包括：
- 第一玻璃基材S1，其线性热膨胀系数为35-60×10-7/℃，
- 下导电层2，优选基于ITO，例如250纳米厚，尤其是热沉积，其方电阻为大约10 Ohms；或者它可以是锑或氟掺杂的氧化锡的层，或包含ITO/ZnO:Al/Ag/ZnO:Al/ITO类型的层堆叠体的多层，各自厚度尤其为ITO 15-20纳米/ZnO:Al 60-80纳米/银3-15纳米/ ZnO:Al 60-80纳米/ITO 15-20纳米，
- 电致变色***3，其结构尤其如下所述，
- 上导电层4, 优选基于ITO，例如110纳米厚，或基于SnO2:F，或者包含其它导电元素的上导电层：这更特别可以涉及将导电层与比它更导电的层和/或多个导电条或线结合。关于更多细节，请参考申请WO-00/57243以加工此类多组分导电层。这种类型的导电层的优选实施方式在于在ITO层(在其上任选地有一个或多个其它导电层)上施用铺设在聚合物片7的表面上的导电线网络6，这种片充当层压中间层并允许在第二基材S2上安装该组件并将电致变色堆叠体连接至电源之一(未显示)，
- 第二玻璃基材S2，其线性热膨胀***也可以为35-60×10-7/℃。
电致变色堆叠体3优选包括：
- 作为对电极，由厚度40至100纳米的氧化铱(水合的)或40至400纳米厚的与或不与其它金属熔合的水合或非水合的氧化镍制成的阳极电致变色材料层EC1，
- 具有电解质功能的层EL，其由通常100纳米厚的氧化钨层、然后通常250纳米厚的选自水合氧化钽、水合氧化硅、水合氧化锆、水合氧化锑的氧化物或它们任何混合物制成的层构成，
- 基于钨WO3或基于钒和钨混合氧化物的阴极电致变色材料层EC2，例如500纳米厚。
从第一基材开始，另一优选的电致变色堆叠体依次包括：
- 基于氧化钨WO3的阴极电致变色材料层，例如300纳米厚的基于氧化钨WO3的阴极电致变色材料层，
- 具有电解质EL功能的层，由通常180纳米厚的氧化钨层和随后通常50纳米厚的氧化硅层构成，
- 镍钨混合氧化物对电极，例如250纳米厚。将这种堆叠体插在通常基于ITO和/或掺杂的氧化锡的两个透明电极之间。在这种类型的堆叠体中，可以***或除去的阳离子优选为锂。
优选借助磁场增强的阴极雾化沉积这组层。或者，其可通过热蒸发或电子流辅助的蒸发、通过激光烧蚀、通过化学气相沉积(CVD)(任选由等离子体或微波辅助)或通过大气压技术，尤其通过经溶胶-凝胶合成的层沉积，尤其通过淬火、喷涂或层流涂布(enduction laminaire)获得。
活性堆叠体3可以借助通过机械方式或通过激光(任选是脉冲的)烧蚀获得的凹槽(gorges)在全部或一部分外周上切割，由此如法国申请FR-2 781 084中所述那样限制漏电。
此外，该器件优选包括与表面2和3接触的第一外周接缝(joint)(2和3传统地是基材S1和S2的内表面的编号)，这种第一接缝适合阻隔外部化学侵蚀。
第二外周接缝(未显示在该图中)与S1、S2的侧面和表面1和4(1和4传统地是基材S1和S2的外表面的编号)接触，以获得与运输工具的安装手段、内外之间的密封性、美观功能和加入增强元件的手段。
该电致变色器件或窗玻璃可用于控制透过安装在建筑物或汽车、火车或飞机类型运输交通工具(例如舷窗)的外部的窗玻璃的日光量。目标是能够限制座舱/房间内部的过度加热，但仅仅在强日照的情况下。
其也可涉及控制穿过窗玻璃的能见度，尤其以使它们模糊，甚至如果需要，阻止所有视野。这可涉及作为在房间、火车、飞机中的内部隔板安装的或作为运输交通工具的侧窗安装的玻璃板。这还涉及用作后视镜的镜子，以完全防止使驾驶员眩目，或用于信息显示板以使信息在需要信息时或间歇出现以最好地引起注意。
本发明的主题因此还是用于建筑物或运输车辆的玻璃窗、隔板、后视镜或信息显示板，它们含有本发明的器件。
下列实施例例证本发明而不限制本发明。
下表1和2提供可用作并入本发明的电致变色器件中的基材的玻璃的组成的若干实例。
这些表中每个显示氧化物的重量含量(以%表示)和标作“CTE”并以10-7/℃表示的热膨胀系数。通常根据标准NF-B30-103测量线性热膨胀系数。
表1
  1 2 3 4 5 6 7
SiO2 (%) 68.2 63.3 64.8 70.5 57 60 60.5
B2O3 (%) - - 10 5.8 4 5 -
Al2O3 (%) 9.3 11.2 14 10 16 18 14.6
MgO (%) 5 8 1.8 2.4 7 8 0.05
CaO (%) 17.5 17.5 2.5 3.1 10 8 11.5
SrO (%) - - - - - - 0.2
BaO (%) - - 2.7 3 6 - 13
Na2O (%) - - 4 5 - 1 -
               
CTE (10-7/℃) 46 47 42 46 46 42 50
表2
  8 9 10 11 12 13 14
SiO2 (%) 59.4 51.9 72 65 74.9 70 64.9
B2O3 (%) 4.5 8 12 3 17 18 9.1
Al2O3 (%) 16.5 20.5 6 13.6 1.7 2.5 16.5
MgO (%) 8.2 8.9 0.4 0.5 0.4 0.5 1.6
CaO (%) 11.4 9.4 1.2 7.9 0.6 1 5.5
SrO (%) - - - 3 - - 1.8
BaO (%) - - 4.3 5.1 - - -
Li2O (%) - - - - - 0.5 -
Na2O (%) - 1.3 2.8 1.1 3.8 0.5 -
K2O (%) - - 0.9 0.9 1.5 6.5 0.6
               
CTE (10-7/℃) 45 41 38 48 38 43 36
通过浮法获得具有这些组成的玻璃基材，随后作为第一基材并入图1中的电致变色器件中，在该基材上沉积电致变色堆叠体。
所得窗玻璃具有与由淬火或硬化钠钙硅玻璃基材制成的电致变色窗玻璃一样好或甚至更好的热力学性能。相反地，在它们中不存在应力，允许切割它们。因此可以在大尺寸基材上沉积构成电致变色堆叠体的层，随后将涂覆基材切割至适合所需尺寸。

Claims (10)

1.包含其线性热膨胀系数为35-60×10-7/℃的第一非淬火玻璃基材(S1)的电致变色器件，所述基材(S1)用包含至少一个透明导电层(2、4)、电致变色材料层(EC2)、离子导电电解质层(EL)和对电极(EC1)的堆叠体涂覆。
2.根据前述权利要求的器件，其中玻璃基材(S1)具有小于或等于50×10-7/℃，甚至小于或等于45×10-7/℃的线性热膨胀系数。
3.根据前述权利要求任一项的器件，其中玻璃基材(S1)具有在下面规定的重量范围内包含如下成分的化学组成：
SiO2                                                   50至82%
B2O3                                                  0至20%
Al2O3                                                 0至22%
MgO                                                  0至10%
CaO                                                   0至15%
SrO                                                    0至5%
BaO                                                   0至15%
CaO+MgO+BaO+SrO                      0至15%,
Na2O                                                 0至6%
K2O                                                   0至8%
Na2O+K2O                                        0至8%  。
4.根据前一权利要求的器件，其中玻璃基材(S1)具有在下面规定的重量范围内包含下列成分的化学组成：
SiO2                                          50至60%
B2O3                                        10至15%
Al2O3                                        10至15%
MgO                                        2至5%
CaO                                         2至5%
SrO                                          0至1%
BaO                                         0至1%
CaO+MgO+BaO+SrO             5至15%
Na2O                                        0至5%
K2O                                         0至5%
Na2O+K2O                               1至6%  。
5.根据前述权利要求任一项的器件，其以从第一基材(S1)开始的顺序或以逆顺序包含：
- 透明导电层(2)，
- 对电极(EC1)，
- 离子导电电解质层(EL)，
- 电致变色材料层(EC2)，
- 第二透明导电层(4)。
6.根据前述权利要求任一项的器件，其中电致变色材料(EC2)基于氧化钨或氧化铱。
7.根据前述权利要求任一项的器件，其中对电极(EL)基于选自钨、镍、铱、铬、铁、钴、铑的元素的氧化物，或基于至少两种这些元素的混合氧化物，特别是镍钨混合氧化物。
8.根据前述权利要求任一项的器件，其中电解质(EL)由形成被电绝缘的离子导体的矿物层构成。
9.根据前述权利要求任一项的器件，其包括第二基材(S2)，该两个基材(S1，S2)被层压或安装为双层玻璃。
10.用于建筑物或运输交通工具的窗玻璃、隔板、后视镜或信号显示板，其包含根据前述权利要求之一的器件。
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CN102639455B (zh) 2016-01-27
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US20120212794A1 (en) 2012-08-23
US8824038B2 (en) 2014-09-02

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