CN112626474A - 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

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CN112626474A
CN112626474A CN202011462541.8A CN202011462541A CN112626474A CN 112626474 A CN112626474 A CN 112626474A CN 202011462541 A CN202011462541 A CN 202011462541A CN 112626474 A CN112626474 A CN 112626474A
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lithium tantalate
film
substrate
magnetron sputtering
sputtering
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CN112626474B (zh
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沈洪雪
汤永康
李刚
姚婷婷
王天齐
金克武
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Glass New Material Innovation Center Anhui Co ltd
CNBM Bengbu Design and Research Institute for Glass Industry Co Ltd
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CNBM Bengbu Design and Research Institute for Glass Industry Co Ltd
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    • 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

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  • Organic Chemistry (AREA)
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  • Mechanical Engineering (AREA)
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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 (3)

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。
2.根据权利要求1所述的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，所述钽酸锂薄膜的厚度为100nm。
3.根据权利要求1所述的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，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。
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