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一种电致变色膜系中的钽酸锂薄膜的制备方法 【EN】Preparation method of lithium tantalate thin film in electrochromic film system

申请(专利)号:CN202011462541.8国省代码:安徽 34
申请(专利权)人:【中文】中建材蚌埠玻璃工业设计研究院有限公司;玻璃新材料创新中心(安徽)有限公司【EN】CHINA BUILDING MATERIALS BENGBU GLASS INDUSTRY DESIGN & RESEARCH INSTITUTE Co.,Ltd.;Glass new material innovation center (Anhui) Co.,Ltd.
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摘要:
【中文】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106Pa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。 【EN】The invention discloses a preparation method of a lithium tantalate film in an electrochromic film system, which comprises the following steps: s1, taking 20 omega of ITO coated glass as a substrate; s2, loading the substrate into a sample rack, and sending the sample rack into a magnetron sputtering coating chamber; taking a lithium tantalate target as a target material; s3, vacuumizing the magnetron sputtering coating cavity until the vacuum degree reaches 106When Pa, heating the substrate at 100-200 ℃; s4, introducing argon into the magnetron sputtering coating cavity, and starting a radio frequency power supply to glow the target; then turning on a direct current power supply, and pre-sputtering the target material in the coupling process of radio frequency and direct current; s5, introducing oxygen after the pre-sputtering is finished, and depositing a lithium tantalate film through magnetron sputtering; s6, after the sample frame is naturally cooled to room temperature, taking out the substrate to obtain a lithium tantalate film; prepared by the methodThe lithium tantalate film has strong controllability and repeatability, and the overall performance of the film system is improved.

主权项:
【中文】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10Pa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。 【EN】1. A preparation method of a lithium tantalate thin film in an electrochromic film system is characterized by comprising the following steps: s1, taking 20 omega of ITO coated glass as a substrate; s2, loading the substrate into a sample rack, and sending the sample rack into a magnetron sputtering coating chamber; taking a lithium tantalate target as a target material; s3, vacuumizing the magnetron sputtering coating cavity until the vacuum degree reaches 10When Pa, heating the substrate at 100-200 ℃; s4, introducing argon into the magnetron sputtering coating cavity, and starting a radio frequency power supply to glow the target; then turning on a direct current power supply, and pre-sputtering the target material in the coupling process of radio frequency and direct current; s5, introducing oxygen after the pre-sputtering is finished, and depositing a lithium tantalate film through magnetron sputtering; and S6, after the sample frame is naturally cooled to room temperature, taking out the substrate to obtain the lithium tantalate film.


说明书

【中文】

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。

【EN】

Preparation method of lithium tantalate thin film in electrochromic film system

Technical Field

The invention relates to the technical field of functional thin films, in particular to a preparation method of a lithium tantalate thin film in an electrochromic film system.

Background

Lithium tantalate material has attracted much attention as a new kind of functional material in recent years, it has high heat-releasing electric coefficient, high Curie temperature, small dielectric constant and other characteristics and has good application prospect, and it has optical performance capable of realizing reversible transformation under low-voltage driving and has attracted much attention, the most direct surface characteristic is different voltage, the color of the material changes accordingly, so it has more and more dominant position in electrochromic material as a main film layer, and its importance has not been neglected. The lithium tantalate film properties determine the overall function of the entire electrochromic film. Therefore, the performance of the film layer is optimized, and the sputtering efficiency is improved, so that the functionality of the whole film group is greatly improved.

Disclosure of Invention

The invention aims to provide a preparation method of a lithium tantalate film in an electrochromic film system.

The technical scheme adopted by the invention for solving the technical problems is as follows:

a preparation method of a lithium tantalate thin film in an electrochromic film system comprises the following steps:

s1, taking 20 omega of ITO coated glass as a substrate;

s2, loading the substrate into a sample rack, and sending the sample rack into a magnetron sputtering coating chamber; taking a lithium tantalate target as a target material;

s3, vacuumizing the magnetron sputtering coating cavity until the vacuum degree reaches 10-6When Pa, heating the substrate at 100-200 ℃;

s4, introducing argon into the magnetron sputtering coating cavity, and starting a radio frequency power supply to glow the target; then turning on a direct current power supply, and pre-sputtering the target material in the coupling process of radio frequency and direct current;

s5, introducing oxygen after the pre-sputtering is finished, and depositing a lithium tantalate film through magnetron sputtering;

and S6, after the sample frame is naturally cooled to room temperature, taking out the substrate to obtain the lithium tantalate film.

Further, the thickness of the lithium tantalate thin film is 100 nm.

Further, in the step S5, during magnetron sputtering, the rf sputtering power is 1250w, the dc sputtering power is 1000w, the argon gas introduction amount is 450sccm, and the time is 120 min.

The invention has the beneficial effects that:

firstly, the magnetron sputtering only carries out the plating of the lithium tantalate film, and the process is simple and has strong controllability.

And secondly, in the film coating process, the problem of low sputtering rate of lithium tantalate can be effectively solved by adopting a radio frequency and direct current coupling mode.

Thirdly, in the process of preparing the film, the substrate is preheated firstly, so that the internal stress of the film can be reduced, and the more stable combination between the film layers is facilitated; meanwhile, after the film is prepared, the film is cooled along with the chamber due to the higher temperature, so that the oxidation of the film is further prevented.

And fourthly, oxygen is introduced in the preparation process, so that the prepared lithium tantalate is prevented from generating a large amount of oxygen defects.

Detailed Description

The invention provides a preparation method of a lithium tantalate film in an electrochromic film system, which comprises the following steps:

s1, taking 20 omega of ITO coated glass as a substrate;

s2, loading the substrate into a sample rack, and sending the sample rack into a magnetron sputtering coating chamber; taking a ceramic lithium tantalate target with the purity of 99.99 percent as a target material;

s3, vacuumizing the magnetron sputtering coating cavity until the vacuum degree reaches 5.0 x 10-6Heating the substrate at 100-200 ℃ under PaC, processing;

s4, introducing argon into the magnetron sputtering coating cavity, and starting a radio frequency power supply to glow the target; then turning on a direct current power supply, bombarding the target material by argon ions in the coupling process of radio frequency and direct current, and carrying out pre-sputtering to achieve the purposes of activating the target material and removing the surface passivation oxide of the target material;

s5, introducing oxygen after the pre-sputtering is finished, and depositing a lithium tantalate film through magnetron sputtering; the radio frequency sputtering power is 1250w, the direct current sputtering power is 1000w, the argon gas introduction amount is 450sccm, and the time is 120 min; the thickness of the lithium tantalate film is 100 nm;

and S6, after the sample frame is naturally cooled to room temperature, taking out the substrate to obtain the lithium tantalate film.

The foregoing is merely a preferred embodiment of the invention and is not intended to limit the invention in any manner; those skilled in the art can make numerous possible variations and modifications to the present teachings, or modify equivalent embodiments to equivalent variations, without departing from the scope of the present teachings, using the methods and techniques disclosed above. Therefore, any simple modification, equivalent replacement, equivalent change and modification made to the above embodiments according to the technical essence of the present invention are still within the scope of the protection of the technical solution of the present invention.

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