CN102636931A - 电致变色层、镀膜件及该镀膜件的制备方法 - Google Patents

电致变色层、镀膜件及该镀膜件的制备方法 Download PDF

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CN102636931A
CN102636931A CN2011100384845A CN201110038484A CN102636931A CN 102636931 A CN102636931 A CN 102636931A CN 2011100384845 A CN2011100384845 A CN 2011100384845A CN 201110038484 A CN201110038484 A CN 201110038484A CN 102636931 A CN102636931 A CN 102636931A
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electrochromic layer
plated film
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张新倍
陈文荣
蒋焕梧
陈正士
黄嘉�
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Hongfujin Precision Industry Shenzhen Co Ltd
Hon Hai Precision Industry Co Ltd
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Hongfujin Precision Industry Shenzhen Co Ltd
Hon Hai Precision Industry Co Ltd
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Priority to TW100105884A priority patent/TW201234920A/zh
Priority to US13/166,323 priority patent/US20120206789A1/en
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Abstract

本发明提供一种电致变色层，具有该电致变色层的镀膜件及该镀膜件的制备方法。该电致变色层为A掺杂的氧化钨层，其中A为钼、铌及钛中的一种或以上，该电致变色层中，A原子百分含量为4～12％，该电致变色层的变色电压为2.1～2.8V。本发明的电致变色层采用掺杂A的氧化钨制成，该氧化钨施加电场及撤去电场的过程中，具有良好的可逆性，可有效地提高镀膜件的使用寿命。

Description

电致变色层、镀膜件及该镀膜件的制备方法
技术领域
本发明涉及一种电致变色层，具有该电致变色层的镀膜件及该镀膜件的制备方法。
背景技术
电致变色材料是在外加电压或者电场的作用下，材料的颜色或者透明度可发生可逆的变化。当外加的电压或者电场消失时，材料的颜色或者透明度回复至初始状态。电致变色薄膜具有记忆功能，广泛地应用于显示器件、调光玻璃、信息存储及外观装饰等领域。现有具有变色功能的镀膜件包括基材及形成于基材上的电致变色薄膜，所述电致变色薄膜通常包括依次层叠的第一透明导电层、电致变色层、离子导电层、离子存储层及第二透明导电层。该第一及第二透明导电层用于施加电场，在外加电场的作用下，所述离子导电层及离子存储层中的离子进入电致变色层，所述电致变色层发生氧化还原反应，从而颜色发生变化。
现有的电致变色层多为有机电致变色材料制成。有机电致变色材料在电场的作用下发生氧化还原反应，使电致变色薄膜的光吸收透过率发生变化而使颜色发生变化。然而，有机电致变色材料的可逆性较差，导致该电致变色层使用的过程中较不稳定，使用寿命较短。
发明内容
有鉴于此，有必要提供一种稳定性高及使用寿命较长的电致变色层。
还有必要提供一种具有上述电致变色层的镀膜件。
另外，还有必要提供一种上述镀膜件的制备方法。
一种电致变色层，该电致变色层为A掺杂的氧化钨层，其中A为钼、铌及钛中的一种或以上，该电致变色层中，A原子百分含量为4～12％，该电致变色层的变色电压为2.1～2.8V，所述电致变色层厚度为500～800nm。
一种镀膜件，包括电致变色层，该电致变色层为A掺杂的氧化钨层，其中A为钼、铌及钛中的一种或以上，该电致变色层中，A的原子百分含量为4～12％，该电致变色层的变色电压为2.1～2.8V。
一种镀膜件的制备方法，包括以下步骤：
提供带有透明导电层的基材、真空镀膜机及合金靶材，该合金靶材为掺杂A的钨，A为钼、铌及钛中至少一种，A原子百分含量为5～15％；
将基材及合金靶材安装于真空镀膜机内；
通入氧气，在基材上镀膜形成电致变色层，该电致变色层的变色电压为2.1～2.8V。
本发明的电致变色层采用掺杂A的氧化钨制成，该氧化钨施加电场及撤去电场的过程中，具有良好的可逆性，可有效地提高电致变色层的使用寿命。
附图说明
图1为本发明一较佳实施例镀膜件的剖视图；
图2是本发明一较佳实施例真空镀膜机的示意图。
主要元件符号说明
镀膜件                    10
基材                      11
第一透明导电层            12
电致变色层                13
离子导体层                14
离子存储层                15
第二透明导电层            16
真空镀膜机                20
镀膜室                    21
合金靶材                    23
具体实施方式
请参阅图1，本发明较佳实施方式的镀膜件10，其包括基材11及依次层叠的第一透明导电层12、电致变色层13、离子导体层14、离子存储层15及第二透明导电层16。所述第一透明导电层12及第二透明导电层16用于对该镀膜件10施加电场，使之发生变色。该离子导体层14及离子存储层15用于在外加电场的作用下为该电致变色层13提供电子及离子，使电致变色层13发生氧化还原反应而变色。
该第一透明导电层12为铟锡氧化物半导体透明导电膜(Indiumtin oxide，ITO)或氧化铝锌透明导电薄膜(AZO)，其可以采用溅射或者蒸镀铟锡氧化物或氧化铝锌形成。
该离子导体层14由LiTaO3或LiNbO3通过溶胶凝胶方式形成。
该离子存储层15由V2O5、NiOx等通过溅射或者溶胶凝胶方式形成。
该第二透明导电层16为铟锡氧化物半导体透明导电膜或氧化铝锌透明导电薄膜玻璃，其可以采用溅射或者蒸镀的方式形成。
该电致变色层13为A掺杂的氧化钨(wolframium oxide，元素符号为WO3)，其中A可为钼(molybdnum，元素符号为Mo)、铌(niobium，元素符号为Nb)、钛(titanium，元素符号为Ti)中的一种或以上；该电致变色层13中A原子百分含量为4～12％，该电致变色层13的厚度可为500～800nm，其变色电压为2.1～2.8V。所述电致变色层13可以采用磁控溅射的方式形成。所述氧化钨掺杂后A，由于A半径与钨的原子半径相近，在形成电致变色层时抑制氧化钨晶粒的长大，晶粒细化，增加了离子的进出通道。此外，由于A的存在破坏部分W-O-W键，在外加电场的作用下更有利于离子的进出，从而降低了临界变色电压。该氧化钨施加电场及撤去电场的过程中，具有良好的可逆性，提高了电致变色层13的稳定性，从而提高了其使用寿命。
该基材11的材质可为不锈钢、铝合金、镁合金、玻璃、陶瓷或塑料。
本发明较佳实施方式的镀膜件10的制备方法，主要包括如下步骤：
采用溅射或者蒸镀铟锡氧化物或氧化铝锌在基材11上形成所述第一透明导电层12。
采用磁控溅射法在第一透明导电层12上形成所述电致变色层13(将结合附图2详细说明)。通过溶胶凝胶方式在电致变色层13上形成离子导体层14。
通过溅射或者溶胶凝胶方式形成所述离子存储层15。
采用溅射或者蒸镀铟锡氧化物或氧化铝锌在基材11上形成所述第一透明导电层12。
请参阅图2，提供带有透明导电层的基材11、真空镀膜机20及合金靶材23，该基材11由不锈钢、铝合金、镁合金、玻璃、陶瓷或塑料制成。该真空镀膜机20设有镀膜室21。所述合金靶材23为掺杂有A的钨材质，其中A可为钼、铌、钛中的一种或以上；该电致变色层13中A的原子百分含量为4～12％。该合金靶材23通过以下方式制得：配置混合粉体，该混合粉体中A占总原子数比例为5-15％，余量为钨；将上述混合粉体在1.0～20×105N的压力下热压制成一坯体，经1700～2000℃烧结1.5～3.0h即可。
清洗以去除基材11表面的污渍，本发明较佳实施例中，该基材11放入无水乙醇中进行超声波清洗，清洗时间可为5～10min。
对经上述处理后的基材11的表面进行氩气等离子体清洗，以进一步去除基材11表面的油污，以及提高基材11表面与后续膜层的结合力。将基材11放入一真空镀膜机20的镀膜室21内，将该镀膜室21抽真空至5.0～3.0×10-5Torr，然后向镀膜室21内通入流量为200～400sccm(标准状态毫升/分钟)的氩气(纯度为99.999％)，并施加-200～-300V的偏压于基材11，对基材11表面进行氩气等离子体清洗，清洗时间为10～20min。
采用磁控溅射法在经氩气等离子体清洗后的基材11的透明导电薄膜上沉积所述电致变色层13。
所述合金靶材23的功率可为2.5～3.5kw，以氧气为反应气体，氧气的流量为50～75sccm，以氩气为工作气体，氩气的流量为300～400sccm，对基材11施加的偏压为-100～-200V，加热所述镀膜室21使基材11的温度为300～400，镀膜时间可为30～60min。所述电致变色层13的厚度可为500～800nm。
对该电致变色层13施加2.1～2.8V的电压时，离子导电层14中的Li+离子及电子进入该电致变色层13中，部分钨从+6价被还原成+5价，该电致变色层13由无色变为蓝色。当撤去外加电场时，所述离子及电子消失，钨从+5价被氧化为+6价，该电致变色层13由蓝色变为无色。
下面通过实施例来对本发明的电致变色层13的制备进行具体说明。
实施例1
本实施例所使用的真空镀膜机20为中频磁控溅射镀膜机，为深圳南方创新真空技术有限公司生产，型号为SM-1100H。
本实施例所使用的基材11的材质为不锈钢；所述合金靶材23中A为钼及钛，其中A中的钼及钛的原子百分含量为钼5％及钛5％，余量的钨粉体，该合金靶材23通过将混合粉体热压制成一坯体，经1800烧结2h制成。
等离子体清洗：氩气流量为400sccm，基材11的偏压为-300V，等离子体清洗时间为10min。
溅镀电致变色层13：合金靶材23的功率为4kw，氧气的流量为60sccm，氩气的流量为300sccm，偏压为-100V，镀膜温度为250，镀膜时间为60min。
由实施例1制得的镀膜件10的电致变色层13厚度为600～700nm，平均值为640nm。在第一透明导电层12及第二透明导电层16之间施加2.4～2.6V的电压时，该电致变色层13由无色变为蓝色。
实施例2
本实施例所使用的真空镀膜机20与实施例1中的相同。
本实施例所使用的基材11的材质为铝合金；所述合金靶材23中A为钼、铌及钛，A各原子百分含量为钼2％、铌1％及钛3％，余量的钨粉体，该合金靶材23通过将混合粉体热压制成一坯体，经1850烧结1.5h制成。
等离子体清洗：氩气流量为400sccm，基材11的偏压为-300V，等离子体清洗时间为10min。
溅镀电致变色层13：合金靶材23的功率为3.5kw，氧气的流量为50sccm，氩气的流量为300sccm，偏压为-150V，镀膜温度为200℃，镀膜时间为60min。
由实施例2制得的镀膜件10的电致变色层13厚度为650～800nm，平均值为655nm，在第一透明导电层12及第二透明导电层16之间施加2.3～2.5V电压时该电致变色层13由无色变为蓝色。
实施例3
本实施例所使用的真空镀膜机20与实施例1中的相同。
本实施例所使用的基材11的材质为玻璃；所述合金靶材23中A为钼、铌及钛，A各原子百分含量为钼5％、铌2％、钛6％，余量为钨，该合金靶材23通过将混合粉体热压制成一坯体，经1900℃烧结2h制成。
等离子体清洗：氩气流量为400sccm，基材11的偏压为-300V，等离子体清洗时间为20min。
溅镀电致变色层13：合金靶材23的功率为4kw，氧气的流量为65sccm，氩气的流量为300sccm，偏压为-120V，镀膜温度为250℃，镀膜时间为60min。
由实施例3制得的镀膜件10的电致变色层13厚度为550～650nm，平均厚度为590nm。在第一透明导电层12及第二透明导电层16之间施加2.1～2.4V电压时该电致变色层13由无色变为蓝色。
实施例4
本实施例所使用的真空镀膜机20与实施例1中的相同。
本实施例所使用的基材11的材质为不锈钢；所述合金靶材23中A为钼、铌及钛，A各原子百分含量为钼3％、铌3％及钛3％，余量为钨，该合金靶材23通过将混合粉体热压制成一坯体，经1950℃烧结1.5h制成。
等离子体清洗：氩气流量为400sccm，基材11的偏压为-300V，等离子体清洗时间为10min。
溅镀电致变色层13：合金靶材23的功率为4.5kw，氧气的流量为60sccm，氩气的流量为300sccm，偏压为-150V，镀膜温度为200℃，镀膜时间为45min。
由实施例3制得的镀膜件10的电致变色层13厚度为500～650nm，平均厚度为590nm。在第一透明导电层12及第二透明导电层16之间施加2.3～2.5V电压时该电致变色层13由无色变为蓝色。
实施例5
本实施例所使用的真空镀膜机20与实施例1中的相同。
本实施例所使用的基材11的材质为玻璃；所述合金靶材23中A为钼及铌，A各原子百分含量为钼5％及铌3％，余量为钨，该合金靶材23通过将混合粉体热压制成一坯体，经1950℃烧结2h制成。
等离子体清洗：氩气流量为400sccm，基材11的偏压为-300V，等离子体清洗时间为60min。
溅镀电致变色层13：合金靶材23的功率为4kw，氧气的流量为65sccm，氩气的流量为300sccm，偏压为-120V，镀膜温度为150℃，镀膜时间为60min。
由实施例5制得的镀膜件10的电致变色层13厚度为500～600nm，平均厚度为565nm。在第一透明导电层12及第二透明导电层16之间施加2.5～2.8V电压时该电致变色层13由无色变为蓝色。
实施例6
本实施例所使用的真空镀膜机20与实施例1中的相同。
本实施例所使用的基材11的材质为玻璃；所述合金靶材23中A为钼，A各原子百分含量为钼15％，余量为钨，该合金靶材23通过将混合粉体热压制成一坯体，经1900℃烧结2h制成。
等离子体清洗：氩气流量为400sccm，基材11的偏压为-300V，等离子体清洗时间为60min。
溅镀电致变色层13：合金靶材23的功率为4kw，氧气的流量为65sccm，氩气的流量为300sccm，偏压为-120V，镀膜温度为150℃，镀膜时间为60min。
由实施例5制得的镀膜件10的电致变色层13厚度为500～600nm，平均厚度为570nm。在第一透明导电层12及第二透明导电层16之间施加2.3～2.6V电压时该电致变色层13由无色变为蓝色。
实施例7
本实施例所使用的真空镀膜机20与实施例1中的相同。
本实施例所使用的基材11的材质为玻璃；所述合金靶材23中A为铌，A各原子百分含量为铌5％，余量为钨，该合金靶材23通过将混合粉体热压制成一坯体，经1800℃烧结2h制成。
等离子体清洗：氩气流量为400sccm，基材11的偏压为-300V，等离子体清洗时间为60min。
溅镀电致变色层13：合金靶材23的功率为3.5kw，氧气的流量为65sccm，氩气的流量为300sccm，偏压为-120V，镀膜温度为150℃，镀膜时间为60min。
由实施例7制得的镀膜件10的电致变色层13厚度为500～600nm，平均厚度为540nm。在第一透明导电层12及第二透明导电层16之间施加2.4～2.7V电压时该电致变色层13由无色变为蓝色。
实施例8
本实施例所使用的真空镀膜机20与实施例1中的相同。
本实施例所使用的基材11的材质为玻璃；所述合金靶材23中A为铌，A各原子百分含量为铌15％，余量为钨，该合金靶材23通过将混合粉体热压制成一坯体，经1950℃烧结2h制成。
等离子体清洗：氩气流量为400sccm，基材11的偏压为-300V，等离子体清洗时间为60min。
溅镀电致变色层13：合金靶材23的功率为4.5kw，氧气的流量为65sccm，氩气的流量为300sccm，偏压为-120V，镀膜温度为150℃，镀膜时间为60min。
由实施例8制得的镀膜件10的电致变色层13厚度为500～600nm，平均厚度为555nm。在第一透明导电层12及第二透明导电层16之间施加2.3～2.5V电压时该电致变色层13由无色变为蓝色。
实施例9
本实施例所使用的真空镀膜机20与实施例1中的相同。
本实施例所使用的基材11的材质为玻璃；所述合金靶材23中A为钛，A各原子百分含量为钛5％，余量为钨，该合金靶材23通过将混合粉体热压制成一坯体，经1700℃烧结2h制成。
等离子体清洗：氩气流量为400sccm，基材11的偏压为-300V，等离子体清洗时间为60min。
溅镀电致变色层13：合金靶材23的功率为3kw，氧气的流量为65sccm，氩气的流量为300sccm，偏压为-120V，镀膜温度为150℃，镀膜时间为60min。
由实施例9制得的镀膜件10的电致变色层13厚度为500～600nm，平均厚度为530nm。在第一透明导电层12及第二透明导电层16之间施加2.5～2.8V电压时该电致变色层13由无色变为蓝色。
实施例10
本实施例所使用的真空镀膜机20与实施例1中的相同。
本实施例所使用的基材11的材质为玻璃；所述合金靶材23中A为钛，A各原子百分含量为钛15％，余量为钨，该合金靶材23通过将混合粉体热压制成一坯体，经1800℃烧结2h制成。
等离子体清洗：氩气流量为400sccm，基材11的偏压为-300V，等离子体清洗时间为60min。
溅镀电致变色层13：合金靶材23的功率为3.5kw，氧气的流量为65sccm，氩气的流量为300sccm，偏压为-120V，镀膜温度为150℃，镀膜时间为60min。
由实施例10制得的镀膜件10的电致变色层13厚度为500～600nm，平均厚度为520nm。在第一透明导电层12及第二透明导电层16之间施加2.3～2.7V，加电压时该电致变色层13由无色变为蓝色。
可以理解，当基材11由导电材料制成时，所述第一透明导电层12可以省略。
本发明较佳实施方式镀膜件10在基材11的表面沉积电致变色层13，该合金靶材23掺杂A，降低了电致变色层13的变色电压，使其具有更加优异的变色性能；且该电致变色层13具有良好的可逆性，可有效地提高镀膜件10的使用寿命。
另外，本领域技术人员还可在本发明权利要求公开的范围和精神内做其它形式和细节上的各种修改、添加和替换。当然，这些依据本发明精神所做的各种修改、添加和替换等变化，都应包含在本发明所要求保护的范围之内。

Claims (10)

1.一种镀膜件，包括电致变色层，其特征在于：该电致变色层为A掺杂的氧化钨层，其中A为钼、铌及钛中的一种或以上，该电致变色层中，A原子百分含量为4～12％，该电致变色层的变色电压为2.1～2.8V。
2.如权利要求1所述的镀膜件，其特征在于：所述电致变色层厚度为500～800nm。
3.如权利要求1所述的镀膜件，其特征在于：所述镀膜件还包括基材及第一透明导电层，所述第一透明导电层形成于基材上，所述电致变色层通过磁控溅射的方式形成于第一透明导电层上。
4.一种电致变色层，其特征在于：该电致变色层为A掺杂的氧化钨层，其中A为钼、铌及钛中的一种或以上，该电致变色层中，A原子百分含量为4～12％，该电致变色层的变色电压为2.1～2.8V。
5.一种镀膜件的制备方法，包括以下步骤：
提供带有透明导电层的基材、真空镀膜机及合金靶材，该合金靶材为掺杂A的钨，A为钼、铌及钛中至少一种，A原子百分含量为5～15％；
将基材及合金靶材安装于真空镀膜机内；
通入氧气，在基材上镀膜形成电致变色层，该电致变色层的变色电压为2.1～2.8V。
6.如权利要求5所述的镀膜件的制备方法，其特征在于：该制备方法还包括于在镀膜之前采用氩气对基材进行等离子清洗的步骤。
7.如权利要求5所述的镀膜件的制备方法，其特征在于：所述形成电致变色层的工艺参数为：所述合金靶材的功率为2.5～3.5kw，氧气的流量为50～75sccm，以氩气为工作气体，氩气的流量为300～400sccm，对基材施加的偏压为-100～-200V，加热使所述镀膜室的温度为300～400℃，镀膜时间为30～60min。
8.如权利要求5所述的镀膜件的制备方法，其特征在于：所述合金靶材的制备采用如下方式实现：所述A粉体与钨粉体形成的混合粉体在1.0～20×105N的压力，热压制成一坯体，经1700～2000℃烧结1.5～3.0h。
9.如权利要求5所述的镀膜件的制备方法，其特征在于：所述基材为不锈钢、铝合金、镁合金、玻璃、陶瓷或塑料。
10.如权利要求5所述的镀膜件的制备方法，其特征在于：所述电致变色层的厚度为500～800nm。
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Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103144380A (zh) * 2013-03-22 2013-06-12 中国南玻集团股份有限公司 三银调光玻璃
CN103145347A (zh) * 2013-03-22 2013-06-12 中国南玻集团股份有限公司 双银调光玻璃
WO2015032200A1 (zh) * 2013-09-05 2015-03-12 华为技术有限公司 一种全固态电致变色复合器件及其制备方法
CN109154756A (zh) * 2016-07-07 2019-01-04 株式会社Lg化学 电致变色装置及其制造方法
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CN111286710A (zh) * 2020-03-30 2020-06-16 天津耀皮工程玻璃有限公司 基于电致变色玻璃用v2o5多层次离子储存层制备方法
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Families Citing this family (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
AR097076A1 (es) * 2013-07-25 2016-02-17 Hpo Assets Llc Películas electrocrómicas y sus métodos relacionados
US20210271145A1 (en) * 2020-02-25 2021-09-02 Sage Electrochromics, Inc. Approaches to modifying a color of an electrochromic stack in a tinted state

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4009935A (en) * 1975-07-11 1977-03-01 Rca Corporation Electrochromic device having a dopant therein to improve its color center absorption characteristics
CN1705045A (zh) * 2004-05-29 2005-12-07 李云平 真空溅射制备柔性导电材料的工艺方法
US20070183066A1 (en) * 1994-05-05 2007-08-09 Donnelly Corporation Signal mirror system for a vehicle
CN101188886A (zh) * 2007-12-14 2008-05-28 北京航空航天大学 一种无机全固态电致变色元件及其制备方法

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4009935A (en) * 1975-07-11 1977-03-01 Rca Corporation Electrochromic device having a dopant therein to improve its color center absorption characteristics
US20070183066A1 (en) * 1994-05-05 2007-08-09 Donnelly Corporation Signal mirror system for a vehicle
CN1705045A (zh) * 2004-05-29 2005-12-07 李云平 真空溅射制备柔性导电材料的工艺方法
CN101188886A (zh) * 2007-12-14 2008-05-28 北京航空航天大学 一种无机全固态电致变色元件及其制备方法

Cited By (14)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103144380B (zh) * 2013-03-22 2016-08-03 中国南玻集团股份有限公司 三银调光玻璃
CN103145347A (zh) * 2013-03-22 2013-06-12 中国南玻集团股份有限公司 双银调光玻璃
CN103144380A (zh) * 2013-03-22 2013-06-12 中国南玻集团股份有限公司 三银调光玻璃
CN103145347B (zh) * 2013-03-22 2016-12-28 中国南玻集团股份有限公司 双银调光玻璃
CN104423114B (zh) * 2013-09-05 2018-03-06 华为技术有限公司 一种全固态电致变色复合器件及其制备方法
CN104423114A (zh) * 2013-09-05 2015-03-18 华为技术有限公司 一种全固态电致变色复合器件及其制备方法
WO2015032200A1 (zh) * 2013-09-05 2015-03-12 华为技术有限公司 一种全固态电致变色复合器件及其制备方法
CN109154756A (zh) * 2016-07-07 2019-01-04 株式会社Lg化学 电致变色装置及其制造方法
CN109154756B (zh) * 2016-07-07 2021-04-27 株式会社Lg化学 电致变色装置及其制造方法
CN111065758A (zh) * 2017-09-08 2020-04-24 依视路国际公司 包括在高离子轰击和低压沉积环境下制备的氧化钨膜的耐用电致变色器件及其制造方法
CN111065758B (zh) * 2017-09-08 2022-06-21 依视路国际公司 包括在高离子轰击和低压沉积环境下制备的氧化钨膜的耐用电致变色器件及其制造方法
CN111286710A (zh) * 2020-03-30 2020-06-16 天津耀皮工程玻璃有限公司 基于电致变色玻璃用v2o5多层次离子储存层制备方法
CN111286710B (zh) * 2020-03-30 2022-08-05 天津耀皮工程玻璃有限公司 基于电致变色玻璃用v2o5多层次离子储存层制备方法
CN113759624A (zh) * 2021-09-09 2021-12-07 宁波伯宇科技有限公司 一种用于制造曲面电致变色镜片的工艺

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