CN112626474B - 一种电致变色膜系中的钽酸锂薄膜的制备方法 - Google Patents

一种电致变色膜系中的钽酸锂薄膜的制备方法 Download PDF

Info

Publication number
CN112626474B
CN112626474B CN202011462541.8A CN202011462541A CN112626474B CN 112626474 B CN112626474 B CN 112626474B CN 202011462541 A CN202011462541 A CN 202011462541A CN 112626474 B CN112626474 B CN 112626474B
Authority
CN
China
Prior art keywords
lithium tantalate
film
substrate
magnetron sputtering
sputtering
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
CN202011462541.8A
Other languages
English (en)
Other versions
CN112626474A (zh
Inventor
沈洪雪
汤永康
李刚
姚婷婷
王天齐
金克武
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.)
Glass New Material Innovation Center Anhui Co ltd
China Building Materials Glass New Materials Research Institute Group Co Ltd
Original Assignee
Glass New Material Innovation Center Anhui Co ltd
China Building Materials Glass New Materials Research Institute Group 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 Glass New Material Innovation Center Anhui Co ltd, China Building Materials Glass New Materials Research Institute Group Co Ltd filed Critical Glass New Material Innovation Center Anhui Co ltd
Priority to CN202011462541.8A priority Critical patent/CN112626474B/zh
Publication of CN112626474A publication Critical patent/CN112626474A/zh
Application granted granted Critical
Publication of CN112626474B publication Critical patent/CN112626474B/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
    • C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
    • C23C14/34—Sputtering
    • C23C14/35—Sputtering by application of a magnetic field, e.g. magnetron 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
    • C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
    • C23C14/08—Oxides
    • G—PHYSICS
    • G02—OPTICS
    • G02F—OPTICAL DEVICES OR ARRANGEMENTS FOR THE CONTROL OF LIGHT BY MODIFICATION OF THE OPTICAL PROPERTIES OF THE MEDIA OF THE ELEMENTS INVOLVED THEREIN; NON-LINEAR OPTICS; FREQUENCY-CHANGING OF LIGHT; OPTICAL LOGIC ELEMENTS; OPTICAL ANALOGUE/DIGITAL CONVERTERS
    • G02F1/00—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics
    • G02F1/01—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics for the control of the intensity, phase, polarisation or colour 
    • G02F1/15—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics for the control of the intensity, phase, polarisation or colour  based on an electrochromic effect
    • G02F1/1514—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics for the control of the intensity, phase, polarisation or colour  based on an electrochromic effect characterised by the electrochromic material, e.g. by the electrodeposited material
    • G02F1/1523—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics for the control of the intensity, phase, polarisation or colour  based on an electrochromic effect characterised by the electrochromic material, e.g. by the electrodeposited material comprising inorganic material

Landscapes

  • Chemical & Material Sciences (AREA)
  • Physics & Mathematics (AREA)
  • Organic Chemistry (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Nonlinear Science (AREA)
  • Inorganic Chemistry (AREA)
  • General Physics & Mathematics (AREA)
  • Optics & Photonics (AREA)
  • Physical Vapour Deposition (AREA)

Abstract

本发明公开一种电致变色膜系中的钽酸锂薄膜的制备方法，包括以下步骤：S1、取20Ω的ITO镀膜玻璃作为衬底；S2、将衬底装入样品架，送入磁控溅射镀膜腔室；以钽酸锂靶为靶材；S3、对磁控溅射镀膜腔室抽真空，当真空度达到10‑ 6Pa时，对衬底进行100～200℃的加热处理；S4、向磁控溅射镀膜腔室内通入氩气，开启射频电源，使靶材起辉；然后打开直流电源，在射频与直流的耦合过程中对靶材进行预溅射；S5、预溅射完毕后通入氧气，通过磁控溅射沉积钽酸锂薄膜；S6、待样品架自然冷却至室温后，取出衬底，得到钽酸锂薄膜；该方法制备得到的钽酸锂薄膜可控性、重复性强，提升膜系的整体性能。

Description

一种电致变色膜系中的钽酸锂薄膜的制备方法
技术领域
本发明涉及功能薄膜技术领域，具体是一种电致变色膜系中的钽酸锂薄膜的 制备方法。
背景技术
钽酸锂材料近年来作为一种新型的功能材料而备受国内外专家的关注，它具有高的热释放电系数，居里温度高，介电常数小等特性而具有良好的应用前景，而其具有的低压驱动下光学性能可实现可逆转变的而备受关注，最直接的表面特征就是电压不同，材料的颜色随之发生变化，故其在电致变色材料中越来越占据主导地位，作为一个主膜层，其重要性已经不容忽视。钽酸锂薄膜性能决定着整个电致变色薄膜的总体功能。因此对膜层的性能进行优化，同时提高其溅射效率等对整个膜组的功能性都有较大的改进。
发明内容
本发明的目的在于提供一种电致变色膜系中的钽酸锂薄膜的制备方法，该方法制备得到的钽酸锂薄膜可控性、重复性强，提升膜系的整体性能。
本发明解决其技术问题所采用的技术方案是：
一种电致变色膜系中的钽酸锂薄膜的制备方法，包括以下步骤：
S1、取20Ω的ITO镀膜玻璃作为衬底；
S2、将衬底装入样品架，送入磁控溅射镀膜腔室；以钽酸锂靶为靶材；
S3、对磁控溅射镀膜腔室抽真空，当真空度达到10-6Pa时，对衬底进行100～200℃的加热处理；
S4、向磁控溅射镀膜腔室内通入氩气，开启射频电源，使靶材起辉；然后打开直流电源，在射频与直流的耦合过程中对靶材进行预溅射；
S5、预溅射完毕后通入氧气，通过磁控溅射沉积钽酸锂薄膜；
S6、待样品架自然冷却至室温后，取出衬底，得到钽酸锂薄膜。
进一步的，所述钽酸锂薄膜的厚度为100nm。
进一步的，所述步骤S5磁控溅射时，射频溅射功率为1250w，直流溅射功率为1000w，氩气通入量为450sccm，时间120min。
本发明的有益效果是：
一、磁控溅射只进行钽酸锂薄膜的镀制，工艺简单，可控性强。
二、在镀膜过程中，采用射频和直流相耦合的方式，可以有效克服钽酸锂溅射速率低的问题。
三、制备薄膜的过程中，先对衬底进行预加热，这样可以减少薄膜的内应力，有利于膜层之间更稳定的结合；同时，薄膜制备完成以后，由于温度仍较高，薄膜进行随腔室冷却，进一步防止薄膜的氧化。
四、在制备过程中通入氧气，避免制备的钽酸锂产生大量的氧缺陷。
具体实施方式
本发明提供一种电致变色膜系中的钽酸锂薄膜的制备方法，包括以下步骤：
S1、取20Ω的ITO镀膜玻璃作为衬底；
S2、将衬底装入样品架，送入磁控溅射镀膜腔室；以纯度为99.99%的陶瓷钽酸锂靶为靶材；
S3、对磁控溅射镀膜腔室抽真空，当真空度达到5.0*10-6Pa时，对衬底进行100～200℃的加热处理；
S4、向磁控溅射镀膜腔室内通入氩气，开启射频电源，使靶材起辉；然后打开直流电源，在射频与直流的耦合过程中，氩离子轰击靶材，进行预溅射，达到活化靶材和去除靶材表面钝化氧化物的目的；
S5、预溅射完毕后通入氧气，通过磁控溅射沉积钽酸锂薄膜；射频溅射功率为1250w，直流溅射功率为1000w，氩气通入量为450sccm，时间120min；钽酸锂薄膜的厚度为100nm；
S6、待样品架自然冷却至室温后，取出衬底，得到钽酸锂薄膜。
以上所述，仅是本发明的较佳实施例而已，并非对本发明作任何形式上的限制；任何熟悉本领域的技术人员，在不脱离本发明技术方案范围情况下，都可利用上述揭示的方法和技术内容对本发明技术方案做出许多可能的变动和修饰，或修改为等同变化的等效实施例。因此，凡是未脱离本发明技术方案的内容，依据本发明的技术实质对以上实施例所做的任何简单修改、等同替换、等效变化及修饰，均仍属于本发明技术方案保护的范围内。

Claims (1)

1.一种电致变色膜系中的钽酸锂薄膜的制备方法，其特征在于，包括以下步骤：
S1、取20Ω的ITO镀膜玻璃作为衬底；
S2、将衬底装入样品架，送入磁控溅射镀膜腔室；以钽酸锂靶为靶材；
S3、对磁控溅射镀膜腔室抽真空，当真空度达到10-6Pa时，对衬底进行100～200℃的加
热处理；
S4、向磁控溅射镀膜腔室内通入氩气，开启射频电源，使靶材起辉；然后打开直流电源，在射频与直流的耦合过程中对靶材进行预溅射；
S5、预溅射完毕后通入氧气，通过磁控溅射沉积钽酸锂薄膜；
S6、待样品架自然冷却至室温后，取出衬底，得到钽酸锂薄膜；
所述钽酸锂薄膜的厚度为100nm；
所述步骤S5磁控溅射时，射频溅射功率为1250w，直流溅射功率为1000w，氩气通入量为450sccm，时间120min。
CN202011462541.8A 2020-12-14 2020-12-14 一种电致变色膜系中的钽酸锂薄膜的制备方法 Active CN112626474B (zh)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN202011462541.8A CN112626474B (zh) 2020-12-14 2020-12-14 一种电致变色膜系中的钽酸锂薄膜的制备方法

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN202011462541.8A CN112626474B (zh) 2020-12-14 2020-12-14 一种电致变色膜系中的钽酸锂薄膜的制备方法

Publications (2)

Publication Number Publication Date
CN112626474A CN112626474A (zh) 2021-04-09
CN112626474B true CN112626474B (zh) 2023-02-17

Family

ID=75312381

Family Applications (1)

Application Number Title Priority Date Filing Date
CN202011462541.8A Active CN112626474B (zh) 2020-12-14 2020-12-14 一种电致变色膜系中的钽酸锂薄膜的制备方法

Country Status (1)

Country Link
CN (1) CN112626474B (zh)

Families Citing this family (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN115125500B (zh) * 2022-06-02 2023-06-16 福建兆元光电有限公司 一种ito机台的复机方法
CN115974552B (zh) * 2023-03-15 2023-06-23 基迈克材料科技（苏州）有限公司 一种磁控溅射用导电钽酸锂靶材的制备方法

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO1996006203A1 (en) * 1994-08-19 1996-02-29 Optical Coating Laboratory, Inc. Electrochromic materials and devices, and method
CN102943244A (zh) * 2012-11-26 2013-02-27 中国民用航空飞行学院 一种钽酸锂薄膜离子束增强沉积制备工艺方法
CN105132874A (zh) * 2015-08-31 2015-12-09 辽宁工业大学 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
CN106637117A (zh) * 2016-12-21 2017-05-10 蚌埠玻璃工业设计研究院 一种高效氮掺杂二氧化钛薄膜的制备方法
CN106835038A (zh) * 2016-12-27 2017-06-13 深圳市三鑫精美特玻璃有限公司 一种制备电致变色薄膜的中频双靶反应溅射工艺及玻璃

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO1996006203A1 (en) * 1994-08-19 1996-02-29 Optical Coating Laboratory, Inc. Electrochromic materials and devices, and method
CN102943244A (zh) * 2012-11-26 2013-02-27 中国民用航空飞行学院 一种钽酸锂薄膜离子束增强沉积制备工艺方法
CN105132874A (zh) * 2015-08-31 2015-12-09 辽宁工业大学 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
CN106637117A (zh) * 2016-12-21 2017-05-10 蚌埠玻璃工业设计研究院 一种高效氮掺杂二氧化钛薄膜的制备方法
CN106835038A (zh) * 2016-12-27 2017-06-13 深圳市三鑫精美特玻璃有限公司 一种制备电致变色薄膜的中频双靶反应溅射工艺及玻璃

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
磁控溅射法制备LiTaO_3薄膜及其结晶性能研究;孙斌玮 等;《半导体光电》;20191231;第40卷(第6期);806-809,814 *

Also Published As

Publication number Publication date
CN112626474A (zh) 2021-04-09

Similar Documents

Publication Publication Date Title
CN112626474B (zh) 一种电致变色膜系中的钽酸锂薄膜的制备方法
CN102912308B (zh) 一种低相变温度二氧化钒薄膜制备工艺
CN104775101B (zh) 一种多孔结构二氧化钒薄膜的制备方法及应用
CN105132877B (zh) 一种二氧化钒薄膜低温沉积方法
CN102251216B (zh) 一种制备掺钨氧化钒薄膜的方法
CN110331366B (zh) 一种二氧化钒基复合薄膜的制备方法
CN110408908B (zh) 一种石墨烯/六硼化镧复合薄膜、制备方法及应用
CN109709737B (zh) 一种电致变色薄膜的制作方法
CN112626459B (zh) 一种电致变色复合膜系中氧化钨层的制备方法
CN106381470A (zh) 一种铜基铌三锡薄膜及其制备方法
CN107022749A (zh) 一种利用分步退火技术制备亚微米级无裂纹铁氧体薄膜的方法
CN108286036B (zh) 一种原位补氧型扫描式电子束气相沉积(ioc-sevd)装置及其方法
CN116103612A (zh) 一种氮化钛薄膜的制作方法
CN109182974A (zh) 一种通过二步快速热退火制备氧化钒薄膜的方法
CN111020506B (zh) 一种基于磁控溅射的在铌酸锂基片上的钛酸锶钡成膜方法
CN116200703A (zh) 一种离子传导层钽酸锂薄膜的制备方法
CN110004419B (zh) 一种利用非平衡磁控溅射技术制备Fe-Si薄膜的方法
CN112553585A (zh) 一种聚甲基丙烯酸甲酯基底介质增透膜及其制备方法
CN102605334A (zh) 一种用于全光器件的Ge-Sb-Se非晶薄膜的制备方法
CN102242339A (zh) 一种氧稳定氟化钇薄膜的制备方法
CN111733388A (zh) 一种ito薄膜的制备方法
CN216639635U (zh) 一种可控晶体结构AlMgB14涂层制备装置
CN105506562A (zh) 一种无氧镀制咖啡色pvd膜的方法
CN117702050A (zh) 一种钨系电致变色薄膜及其制备方法
JPS63243261A (ja) 低抵抗透明導電膜の製造方法

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
CB02 Change of applicant information

Address after: 233000 1047 Tu Shan Road, Yuhui District, Bengbu, Anhui

Applicant after: China Building Materials Glass New Materials Research Institute Group Co.,Ltd.

Applicant after: Glass new material innovation center (Anhui) Co.,Ltd.

Address before: 233000 1047 Tu Shan Road, Yuhui District, Bengbu, Anhui

Applicant before: CHINA BUILDING MATERIALS BENGBU GLASS INDUSTRY DESIGN & RESEARCH INSTITUTE Co.,Ltd.

Applicant before: Glass new material innovation center (Anhui) Co.,Ltd.

CB02 Change of applicant information
GR01 Patent grant
GR01 Patent grant