CN115261792B - 一种电致变色涂层的制备方法 - Google Patents

一种电致变色涂层的制备方法 Download PDF

Info

Publication number
CN115261792B
CN115261792B CN202210822870.1A CN202210822870A CN115261792B CN 115261792 B CN115261792 B CN 115261792B CN 202210822870 A CN202210822870 A CN 202210822870A CN 115261792 B CN115261792 B CN 115261792B
Authority
CN
China
Prior art keywords
coating
film
electrochromic
starting
preparation
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Active
Application number
CN202210822870.1A
Other languages
English (en)
Other versions
CN115261792A (zh
Inventor
谷松
刘大光
季璐
聂旭
马佳伟
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Jinxi Research Institute Of Chemical Industry Co ltd
Original Assignee
Jinxi Research Institute Of Chemical Industry Co ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Jinxi Research Institute Of Chemical Industry Co ltd filed Critical Jinxi Research Institute Of Chemical Industry Co ltd
Priority to CN202210822870.1A priority Critical patent/CN115261792B/zh
Publication of CN115261792A publication Critical patent/CN115261792A/zh
Application granted granted Critical
Publication of CN115261792B publication Critical patent/CN115261792B/zh
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Classifications

    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
    • C23C14/08—Oxides
    • C23C14/083—Oxides of refractory metals or yttrium
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/0021—Reactive sputtering or evaporation
    • C23C14/0036—Reactive sputtering
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
    • C23C14/34—Sputtering
    • C23C14/3464—Sputtering using more than one target
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
    • C23C14/50—Substrate holders
    • C23C14/505—Substrate holders for rotation of the substrates

Landscapes

  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Electrochromic Elements, Electrophoresis, Or Variable Reflection Or Absorption Elements (AREA)

Abstract

本发明提供电致变色涂层的制备方法。本发明采用的涂层是以PC板材为基材，通过磁控溅射法涂覆ITO导电膜(膜厚100nm，方阻20Ω/sq)，GaO3与NbOx膜层制得。本发明的涂层稳定性好，制备简单，能有效减少电变色层的漏电流，缩短相应时间。

Description

一种电致变色涂层的制备方法
技术领域
本发明涉及一种镀在聚碳酸酯材料上的涂层，特别是涉及一种在聚碳酸酯材料上电致变色的涂层。
背景技术
目前，电致变色的产品不断的被制造研发，带来了极大的生产效益，这些产品包括：波音787飞机弦窗所使用的可调节光透过率、无窗影的电控弦窗、保时捷Nbycan GTS系列等所使用全景天窗、后视镜以及航天器热控涂层、电致变色显示器、电子标签及电子纸。其中将电致变色材料制备出的智能窗可广泛应用于大厦商场外的建筑玻璃上，及汽车玻璃挡板上减少能源的消耗。在热气候时，通过施加合适的电压用以调节智能窗的光透过率，以减少室内太阳光的强度，从而减少室内的温度，并且可减少由于强烈太阳光所造成对人体的不适。目前来讲，电致变色涂层中较为常用的为WO3薄膜，相较于其它电致变色薄膜而言，有较为优越的综合性能，但也存在循环稳定性差、着色效率较小等缺点。目前用来改进与提升WO3薄膜的性能的方法包括：(1)掺杂与退火结晶，虽然能提高薄膜的循环寿命，但却使响应时间等相关的电致变色性能变差。(2)引入纳米结构，虽使WO3薄膜变色性能提高的同时，又保证了良好的化学稳定性，但制作工艺变复杂了。目前，对于WO3，有必要增添一种更方便有效的制备方法，去进一步提升WO3薄膜的电致变色相关性能参数。这对电致变色未来的发展，以及工业化有着重要的意义。由于NbOx具有稳定性好，制备简单，能有效减少电变色层的漏电流等一系列的优点，具有十分重要的意义。
发明内容
本发明的目的在于，在聚碳酸酯基材上，镀上一系列涂层，有效减少电致变色层的漏电流。
为达到上述目的，本发明的技术方案是这样实现的：
所述涂层制备方法为：
1)在PC基材上，涂覆ITO导电膜(膜厚100nm，方阻20Ω/sq)。
2)安装好Ga靶，然后启动冷凝水装置，然后启动分子泵，当真空腔的压力在6×10- 4Pa以下，打开氩气阀，调节氩气流量为50Sccm，氧气流量15Sccm。设置样品台的旋转速度为20r/min。在150GA功率，溅射1h。。
3)安装好Nb靶，然后启动冷凝水装置，然后启动分子泵，当真空腔的压力在6×10- 4Pa以下，打开氩气阀，调节氩气流量为50Sccm，氧气流量20Sccm。设置样品台的旋转速度为20r/min。在150w功率，溅射1h。
本发明有益效果：
由于NbOx具有稳定性好，制备简单，能有效减少电变色层的漏电流，缩短相应时间。
具体实施方式
下面结合实施例对本发明进行详细说明：
实施例1：
1)在PC基材上，涂覆ITO导电膜(膜厚100nm，方阻20Ω/sq)。
2)安装好Ga靶，然后启动冷凝水装置，启动分子泵，当真空腔的压力在6×10-4Pa以下，打开氩气阀，调节氩气流量为50Sccm，氧气流量15Sccm。设置样品台的旋转速度为20r/min。在150W功率，溅射1h。。
3)安装好Nb靶，然后启动冷凝水装置，启动分子泵，当真空腔的压力在6×10-4Pa以下，打开氩气阀，调节氩气流量为50Sccm，氧气流量20Sccm。设置样品台的旋转速度为20r/min。在150W功率，溅射1h。
实施例2
将实施例1中的氧气流量更改为15Sccm。在150W功率，溅射1h。
实施例3
将实施例1中的氧气流量更改为10Sccm。在150W功率，溅射1h。
通过采用计时电流法，以及紫外分光光度计共同测量，得出薄膜在指定光波长的光透过率以及电流随时间的变化。使用电化学工作站对制备样品施加一个方波信号，此时薄膜或器件便会发生着色以及褪色的反应，测试中紫外分光光度计记录着薄膜或器件的光透过率与时间的关系，而电化学工作站则记录着电流与时间的关系，透过这些关系可得出薄膜或器件的输入输出电荷量，响应时间与着色效率等一些列电致变色薄膜或器件的重要性能指标。
表1样品的原子氧侵蚀率测试结果
样品名称 NbOx膜 实施例1 实施例2 实施例3
显色相应时间 9 6 7 7
褪色相应时间 9 5 6 7
从表1性能测试结果可知，实施例1涂层，NbOx显色相应时间、褪色相应时间最少，并且薄膜的着色效率得到明显的提高。
以上所述仅为本发明的较佳实施例而已，并不用以限制本发明，凡在本发明的精神和原则之内，所作的任何修改、等同替换、改进、不同用途等，均应包含在本发明的保护范围之内。

Claims (1)

1.电致变色涂层的制备方法，其特征在于：包括以下步骤：1)在PC基材上，涂覆ITO导电膜，所述导电膜的膜厚为100nm，方阻为20Ω/sq；2)安装好Ga靶，然后启动冷凝水装置，启动分子泵，当真空腔的压力在6×10-4Pa以下，打开氩气阀，调节氩气流量为50Sccm，氧气流量15Sccm；设置样品台的旋转速度为20r/min；在150W功率，溅射1h，形成GaO3膜；3)更换成Nb靶，然后启动冷凝水装置，启动分子泵，当真空腔的压力在6×10-4Pa以下，打开氩气阀，调节氩气流量为50Sccm，氧气流量20Sccm；设置样品台的旋转速度为20r/min；在150W功率，溅射1h，形成NbOx膜。
CN202210822870.1A 2022-07-05 2022-07-05 一种电致变色涂层的制备方法 Active CN115261792B (zh)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN202210822870.1A CN115261792B (zh) 2022-07-05 2022-07-05 一种电致变色涂层的制备方法

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN202210822870.1A CN115261792B (zh) 2022-07-05 2022-07-05 一种电致变色涂层的制备方法

Publications (2)

Publication Number Publication Date
CN115261792A CN115261792A (zh) 2022-11-01
CN115261792B true CN115261792B (zh) 2023-10-13

Family

ID=83764104

Family Applications (1)

Application Number Title Priority Date Filing Date
CN202210822870.1A Active CN115261792B (zh) 2022-07-05 2022-07-05 一种电致变色涂层的制备方法

Country Status (1)

Country Link
CN (1) CN115261792B (zh)

Citations (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4832463A (en) * 1987-09-08 1989-05-23 Tufts University Thin film ion conducting coating
CN1397661A (zh) * 2001-06-26 2003-02-19 三井金属矿业株式会社 高电阻透明导电膜用溅射靶及高电阻透明导电膜的制造方法
JP2005099756A (ja) * 2003-08-21 2005-04-14 Asahi Glass Co Ltd 反射防止膜
JP2007187993A (ja) * 2006-01-16 2007-07-26 Bridgestone Corp エレクトロクロミック素子及びその製造方法
CN106249500A (zh) * 2016-08-25 2016-12-21 北京工业大学 一种基于非晶态‑纳米晶复合结构的柔性电致变色器件及其制备方法
CN107632479A (zh) * 2017-11-07 2018-01-26 宁波祢若电子科技有限公司 一种改进型电致变色汽车后视镜镜片
WO2020076798A1 (en) * 2018-10-08 2020-04-16 Board Of Regents, The University Of Texas System Porous electrochromic niobium oxide films and methods of making and use thereof
CN112285982A (zh) * 2020-11-06 2021-01-29 哈尔滨工业大学 一种以硅酸铝锂为电解质层的全固态电致变色器件及其制备方法
CN112992408A (zh) * 2021-01-28 2021-06-18 中国乐凯集团有限公司 柔性复合透明导电膜及其制备方法和器件

Family Cites Families (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US9759975B2 (en) * 2010-04-30 2017-09-12 View, Inc. Electrochromic devices
US20130095292A1 (en) * 2010-10-29 2013-04-18 Cardinal Solar Technologies Company TCO Coating and Coated Substrate for High Temperature Applications

Patent Citations (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4832463A (en) * 1987-09-08 1989-05-23 Tufts University Thin film ion conducting coating
CN1397661A (zh) * 2001-06-26 2003-02-19 三井金属矿业株式会社 高电阻透明导电膜用溅射靶及高电阻透明导电膜的制造方法
JP2005099756A (ja) * 2003-08-21 2005-04-14 Asahi Glass Co Ltd 反射防止膜
JP2007187993A (ja) * 2006-01-16 2007-07-26 Bridgestone Corp エレクトロクロミック素子及びその製造方法
CN106249500A (zh) * 2016-08-25 2016-12-21 北京工业大学 一种基于非晶态‑纳米晶复合结构的柔性电致变色器件及其制备方法
CN107632479A (zh) * 2017-11-07 2018-01-26 宁波祢若电子科技有限公司 一种改进型电致变色汽车后视镜镜片
WO2020076798A1 (en) * 2018-10-08 2020-04-16 Board Of Regents, The University Of Texas System Porous electrochromic niobium oxide films and methods of making and use thereof
CN112285982A (zh) * 2020-11-06 2021-01-29 哈尔滨工业大学 一种以硅酸铝锂为电解质层的全固态电致变色器件及其制备方法
CN112992408A (zh) * 2021-01-28 2021-06-18 中国乐凯集团有限公司 柔性复合透明导电膜及其制备方法和器件

Also Published As

Publication number Publication date
CN115261792A (zh) 2022-11-01

Similar Documents

Publication Publication Date Title
CN103246119B (zh) 一种wo3电致变色薄膜的制备方法
CN107085339B (zh) 一种全固态电致变色器件的制备方法
CN101622721B (zh) 太阳能电池用透明电极及其制造方法
CN105132874B (zh) 一种直流/射频共溅射法制备高浓度梯度azo单晶导电薄膜的方法
CN100485082C (zh) 一种直流磁控共溅射法制备ZnO:Al透明导电薄膜的方法
CN111574071B (zh) 一种高透过宽色系盖板玻璃的制备方法
CN104178731B (zh) 一种电致变色wo3薄膜的可控制备方法
CN101619445A (zh) 一种透明导电薄膜材料的制备方法
CN101985740A (zh) 一种铝掺氧化锌透明导电薄膜的退火方法
CN110045558A (zh) 铝酸锂固态离子传导层及其制备方法与含该固态离子传导层的全固态电致变色器件
CN110791740B (zh) 一种高性能zif-l/二氧化钒复合薄膜的制备方法
CN110129850B (zh) 一种亚铁氰化铁薄膜的分步沉积制备方法
CN115261792B (zh) 一种电致变色涂层的制备方法
CN109267028B (zh) 一种镍锌氧化合物光电薄膜及其制备方法
CN107315298B (zh) 一种褐色电致变色电荷存储电极及制备方法
CN103924191A (zh) 在基片上镀制ito薄膜的方法
CN106893984B (zh) 增强可见光波段透射的掺锡氧化铟基复合薄膜的制备方法
CN104630731A (zh) 一种电致变色器件的制备方法
CN2789934Y (zh) 大面积太阳电池纳米透明导电膜制备专用加热装置
CN116377405A (zh) 一种基于Ta元素掺杂的VO2薄膜的制备方法
CN105132875B (zh) 一种扩散法制备高浓度梯度azo单晶导电薄膜的方法
CN106637204A (zh) Ag/ZnO/Mg光电透明导电薄膜的沉积方法
CN109037390A (zh) 一种锡酸镉基透明导电膜、其生产工艺及太阳能电池
CN107293605A (zh) 太阳能电池背电极和太阳能电池及其制备方法
CN102456768A (zh) 含有ZnO:Al窗口层的ZnO/SnS太阳能电池元件的制备方法

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
GR01 Patent grant
GR01 Patent grant