CN112626459B - 一种电致变色复合膜系中氧化钨层的制备方法 - Google Patents

一种电致变色复合膜系中氧化钨层的制备方法 Download PDF

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CN112626459B
CN112626459B CN202011462996.XA CN202011462996A CN112626459B CN 112626459 B CN112626459 B CN 112626459B CN 202011462996 A CN202011462996 A CN 202011462996A CN 112626459 B CN112626459 B CN 112626459B
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tungsten oxide
sputtering
substrate
magnetron sputtering
oxide film
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CN112626459A (zh
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沈洪雪
汤永康
王天齐
金克武
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China Building Materials Glass New Materials Research Institute Group 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
    • C23C14/06—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
    • C23C14/35—Sputtering by application of a magnetic field, e.g. magnetron sputtering

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Abstract

本发明公开一种电致变色复合膜系中氧化钨层的制备方法，包括以下步骤：S1、选用电阻率为20欧姆的ITO镀膜玻璃作为为衬底；S2、将衬底装入样品架，送入磁控溅射镀膜腔室中；S3、对磁控溅射镀膜腔室抽真空，使真空度达到8.0*10‑ 6Pa；S4、当真空度达到10‑6Pa时，对衬底进行加热至300℃，并通入氩气，同时开启直流电源，使靶材进行预溅射；S5、预溅射完毕后，通入氧气，溅射氧化钨薄膜；S6、溅射完毕后，待磁控溅射镀膜腔室降温至室温后，取出氧化钨薄膜；该方法制备得到的氧化钨薄膜具有膜层厚度均匀、性能优良稳定的特点，且工艺简单、可控性强。

Description

一种电致变色复合膜系中氧化钨层的制备方法
技术领域
本发明涉及功能薄膜制备技术领域，具体是一种电致变色复合膜系中氧化钨层的制备方法。
背景技术
电致变色材料分为无机电致变色材料和有机电致变色材料。因其在低压驱动下光学性能可实现可逆转变而备受关注，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，其中无机电致变色材料的典型代表是几种电致变色膜系的复合，使得材料达到最佳的变色效果，而复合膜系中的核心膜层是氧化钨，氧化钨薄膜性能的好坏直接决定着电致变色薄膜的总体性能。
发明内容
本发明的目的在于提供一种电致变色复合膜系中氧化钨层的制备方法，该方法制备得到的氧化钨薄膜具有膜层厚度均匀、性能优良稳定的特点，且工艺简单、可控性强。
本发明解决其技术问题所采用的技术方案是：
一种电致变色复合膜系中氧化钨层的制备方法，包括以下步骤：
S1、选用电阻率为20欧姆的ITO镀膜玻璃作为为衬底；
S2、将衬底装入样品架，送入磁控溅射镀膜腔室中；
S3、对磁控溅射镀膜腔室抽真空，使真空度达到8.0*10-6Pa；
S4、当真空度达到10-6Pa时，对衬底进行加热至300℃，并通入氩气，同时开启直流电源，使靶材进行预溅射；
S5、预溅射完毕后，通入氧气，溅射氧化钨薄膜；
S6、溅射完毕后，待磁控溅射镀膜腔室降温至室温后，取出氧化钨薄膜。
进一步的，步骤S5溅射时通入的氧气由10sccm～20sccm渐变。
进一步的，磁控溅射时的功率为1250w，氩气通入量保持为450sccm。
进一步的，制备得到的氧化钨薄膜厚度为100～200nm。
本发明的有益效果是：
一、磁控溅射只进行氧化钨薄膜的镀制，工艺简单，可控性强；
二、溅射之前，先对衬底进行加热至300℃，可以减少薄膜的内应力，有利于膜层之间更稳定的结合；
三、溅射完毕后，由于温度较高，待薄膜跟随磁控溅射镀膜腔室降温至室温后再取出，能够防止薄膜的氧化；
四、溅射时氧气由10sccm～20sccm渐变，可以得到符合电致变色使用、具有氧缺陷的斜方相氧化钨薄膜。
具体实施方式
本发明提供一种电致变色复合膜系中氧化钨层的制备方法，包括以下步骤：
S1、选用电阻率为20欧姆的ITO镀膜玻璃作为为衬底；
S2、将衬底装入样品架，送入磁控溅射镀膜腔室中；
S3、对磁控溅射镀膜腔室抽真空，使真空度达到8.0*10-6Pa；
S4、当真空度达到8.0*10-6Pa时，对衬底进行加热至300℃，并通入氩气，同时开启直流电源，使靶材进行30分钟预溅射以去除靶材表面的氧化钨并激活靶材；
S5、预溅射完毕后，通入10sccm～20sccm渐变的氧气，溅射氧化钨薄膜；磁控溅射时的功率为1250w，氩气通入量保持为450sccm；循环10次，得到的氧化钨薄膜厚度为100～200nm；
S6、溅射完毕后，待磁控溅射镀膜腔室降温至室温后，取出氧化钨薄膜。
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)

1.一种电致变色复合膜系中氧化钨层的制备方法，其特征在于，包括以下步骤： S1、选用电阻率为20欧姆的ITO镀膜玻璃作为为衬底； S2、将衬底装入样品架，送入磁控溅射镀膜腔室中； S3、对磁控溅射镀膜腔室抽真空，使真空度达到8.0*10-6Pa； S4、当真空度达到10-6Pa时，对衬底进行加热至300℃，并通入氩气，同时开启直流电源，使靶材进行预溅射； S5、预溅射完毕后，通入氧气，溅射氧化钨薄膜； S6、溅射完毕后，待磁控溅射镀膜腔室降温至室温后，取出氧化钨薄膜；
步骤S5溅射时通入的氧气通入量由10sccm～20sccm渐变，磁控溅射时的功率为1250w，氩气通入量保持为450sccm；
制备得到的氧化钨薄膜厚度为100～200nm。
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Citations (4)

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Publication number Priority date Publication date Assignee Title
TW434704B (en) * 1999-06-11 2001-05-16 Univ Nat Yunlin Sci & Tech Device of amorphous WO3 ion sensitive field effect transistor (ISFET) and method for making the same
CN103246119A (zh) * 2013-05-10 2013-08-14 南京理工大学 一种wo3电致变色薄膜的制备方法
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
CN110642526A (zh) * 2019-09-16 2020-01-03 中国科学院宁波材料技术与工程研究所 一种氧化钨电致变色薄膜的制备方法

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
TW434704B (en) * 1999-06-11 2001-05-16 Univ Nat Yunlin Sci & Tech Device of amorphous WO3 ion sensitive field effect transistor (ISFET) and method for making the same
CN103246119A (zh) * 2013-05-10 2013-08-14 南京理工大学 一种wo3电致变色薄膜的制备方法
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
CN110642526A (zh) * 2019-09-16 2020-01-03 中国科学院宁波材料技术与工程研究所 一种氧化钨电致变色薄膜的制备方法

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