CN113930723A - 一种高度择优取向Magnéli相Ti6O11透明导电薄膜及其制备方法和应用 - Google Patents

一种高度择优取向Magnéli相Ti6O11透明导电薄膜及其制备方法和应用 Download PDF

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CN113930723A
CN113930723A CN202111200705.4A CN202111200705A CN113930723A CN 113930723 A CN113930723 A CN 113930723A CN 202111200705 A CN202111200705 A CN 202111200705A CN 113930723 A CN113930723 A CN 113930723A
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乔文涛
李明
王康佳
宗海涛
潘靖
殷月红
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Abstract

本发明涉及一种高度择优取向Magnéli相Ti6O11透明导电薄膜及其制备方法和应用，该制备方法的步骤如下：采用脉冲激光沉积法，以石英玻璃作为衬底、TiO2作为靶材，靶材和衬底之间的间距保持在4‑8cm，激光束以45°的入射角度照射在靶材表面，先将腔室抽真空为1×10‑3‑5×10‑3 Pa，然后加热衬底温度至200‑700℃，再继续抽真空为1×10‑4‑5×10‑4 Pa，接着通氧气，控制氧流量为10sccm，调节氧分压为5‑10Pa；先预溅射5min，去除靶材表面氧化物后再开始向衬底溅射，结束后原位退火至室温，即生成沉积在石英玻璃衬底上的Magnéli相Ti6O11透明导电薄膜，其中生长速率为2‑12 nm/min。该薄膜材料为纯Ti6O11Magnéli相且具有高度择优取向性，同时具有良好的导电性和可见区及近红外光区的透光率。

Description

一种高度择优取向Magnéli相Ti6O11透明导电薄膜及其制备方 法和应用
技术领域
本发明涉及透明导电薄膜技术领域，尤其涉及一种高度择优取向Magnéli相Ti6O11透明导电薄膜及其制备方法和应用。
背景技术
Magnéli相亚氧化钛TinO2n-1(4≤n≤10)自60年前发现以来也引起了广泛关注。Magnéli相亚氧化钛TinO2n-1以金红石相TiO2结构为基础，每间隔n层TiO2结构，存在一个氧缺失层TiO。氧缺陷层的存在降低了TinO2n-1的禁带宽度，使其具有良好的导电性，Magnéli相亚氧化钛的电导率要比TiO2的电导率高出几个数量级。TiO2层的存在又使Magnéli相亚氧化钛保留了金红石相TiO2优良的化学稳定性和良好的耐磨性。这些优点使Magnéli相亚氧化钛在燃料电池、污水处理、电极材料等方面显示了巨大的应用潜力。
目前，Magnéli相亚氧化钛薄膜主要有溶胶-凝胶法、物理气相沉积法、化学气相沉积法和等离子喷涂法等制备方法。根据文献报道，制备出的Magnéli相亚氧化钛薄膜多为TiO2(如锐钛矿相和金红石相)和多种Magnéli相(如Ti4O7、Ti5O9、Ti6O11等)的混合相薄膜，纯Magnéli相亚氧化钛薄膜的制备难度较大，目前还未见相关报道。
因此，本发明提出一种高度择优取向Magnéli相Ti6O11透明导电薄膜的制备方法，该薄膜材料为纯Ti6O11Magnéli相，其生长方式具有高度择优取向性，同时具有良好的导电性和可见区及近红外光区的透光率。为宽谱太阳能电池、表面气敏传感器、显示屏等提供了备选材料。
发明内容
解决的技术问题：针对现有技术存在的缺点，本发明提供一种高度择优取向Magnéli相Ti6O11透明导电薄膜及其制备方法和应用，该薄膜材料为纯Ti6O11Magnéli相且具有高度择优取向性，同时具有良好的导电性和可见区及近红外光区的透光率。
技术方案：一种高度择优取向Magnéli相Ti6O11透明导电薄膜的制备方法，步骤如下：
(1)石英玻璃预处理：将石英玻璃分别在丙酮、无水乙醇、去离子水溶液中超声清洗10min，最后用氮气干燥，备用；
(2)沉积准备：采用脉冲激光沉积法，以石英玻璃作为衬底、TiO2作为靶材，靶材和衬底之间的间距保持在4-8cm，激光束以45°的入射角度照射在靶材表面，先将腔室抽真空为1×10-3-5×10-3Pa，然后加热衬底温度至200-700℃，再继续抽真空为1×10-4-5×10-4Pa，接着通氧气，控制氧流量为10sccm，调节氧分压为5-10Pa；
(3)沉积：先预溅射5min，去除靶材表面氧化物后再开始向衬底溅射，结束后原位退火至室温，即生成沉积在石英玻璃衬底上的Magnéli相Ti6O11透明导电薄膜，其中生长速率为2-12nm/min。
上述所述的脉冲激光沉积法的设置参数为脉冲激光波长248nm、脉冲宽度25ns、脉冲频率5Hz、输出脉冲能量为200-300mJ。
上述所述的TiO2靶材的纯度为99.99％、直径为40mm、厚度为3mm。
上述所述的生成的Magnéli相Ti6O11透明导电薄膜的厚度为30～200nm。
由上述所述的制备方法制备得到的高度择优取向Magnéli相Ti6O11透明导电薄膜。
上述所述的透明导电薄膜为纯Magnéli相Ti6O11透明导电薄膜。
上述所述的纯Magnéli相Ti6O11透明导电薄膜在(-204)晶面有高度的择优取向性。
由上述所述的制备方法制备得到的高度择优取向Magnéli相Ti6O11透明导电薄膜在宽谱太阳能电池、表面气敏传感器或显示屏中的应用。
本发明的高度择优取向Magnéli相Ti6O11透明导电薄膜作为宽谱太阳电池的窗口层，在可见光近红外的高透过率和优良的电学性能对提高宽谱太阳能电池转化效率有重要作用，同时作用在宽谱太阳电池的前电极，能起到收集电流，增透减反的作用。
也可利用本发明的高度择优取向Magnéli相Ti6O11透明导电薄膜优良的导电性对气体表面吸附产生的变化，制造表明气敏传感器。
有益效果：本发明提供的一种高度择优取向Magnéli相Ti6O11透明导电薄膜及其制备方法和应用，具有以下有益效果：
1.本发明的制备方法，通过在玻璃衬底沉积形成透明导电薄膜，该薄膜为纯Ti6O11Magnéli相薄膜材料；
2.本发明的纯Magnéli相Ti6O11透明导电薄膜在可见区及近红外光区具有很高的透光率；
3.本发明的纯Magnéli相Ti6O11透明导电薄膜在(-204)晶面有高度的择优取向性，此结构有利于在该薄膜之上进一步引入其他功能薄膜，也有利于通过掺杂进一步提高其导电及透光性能。
附图说明
图1为实施例1制备得到的Magnéli相Ti6O11透明导电薄膜的XRD图。
图2为实施例1制备得到的Magnéli相Ti6O11透明导电薄膜的可见光及近红外光区透射图。
图3为实施例2制备得到的Magnéli相Ti6O11透明导电薄膜的XRD图。
图4为实施例2制备得到的Magnéli相Ti6O11透明导电薄膜的可见光及近红外光区透射图。
图5为实施例3制备得到的Magnéli相Ti6O11透明导电薄膜的XRD图。
图6为实施例3制备得到的Magnéli相Ti6O11透明导电薄膜的可见光及近红外光区透射图。
图7为实施例4制备得到的Magnéli相Ti6O11透明导电薄膜的XRD图。
图8为实施例4制备得到的Magnéli相Ti6O11透明导电薄膜的可见光及近红外光区透射图。
具体实施方式
以下实施例中所用脉冲激光由KrF准分子激光器提供，激光器型号：CoherentCOMPex Pro-102F，厂家：美国Coherent公司；所用TiO2为靶材，纯度99.99％，直径40mm，厚度3mm，厂家：河北罗鸿科技有限公司；所用石英玻璃衬底尺寸1cm×1cm，厚度0.5mm，石英衬底含99.5％以上的SiO2，有Na、Ga、K等杂质。
实施例1
该实施例提供一种高度择优取向Magnéli相Ti6O11透明导电薄膜的制备方法，步骤如下：采用脉冲激光沉积法生长Magnéli相Ti6O11薄膜层，脉冲激光波长248nm、脉冲宽度25ns、脉冲频率5Hz、输出脉冲能量为300mJ；使用TiO2为靶材，纯度99.99％，直径40mm，厚度3mm；采用石英玻璃作为衬底，石英玻璃分别在丙酮、无水乙醇、去离子水溶液中超声清洗10min，最后用氮气干燥。
靶材和衬底之间的间距保持在6cm，激光束以45°的入射角度照射在靶材表面。生长时先将腔室抽真空为5×10-3Pa；然后加热衬底温度至300℃；再继续抽真空为5×10-4Pa；接着通氧气，控制氧流量为10sccm，调节氧分压为5Pa；沉积前先预溅射5min，去除靶材表面氧化物，再开始向衬底溅射，结束后原位退火至室温，生成沉积在石英玻璃衬底上的Magnéli相Ti6O11透明导电薄膜，生长速率为10nm/min，Magnéli相Ti6O11透明导电薄膜的厚度为50nm。
实施例2
实施例2与实施例1的区别在于沉积在石英玻璃衬底上的Magnéli相Ti6O11透明导电薄膜的厚度为100nm。
实施例3
实施例3与实施例1的区别在于加热衬底温度至650℃。
实施例4
实施例4与实施例1的区别在于加热衬底温度至650℃，且沉积在石英玻璃衬底上的Magnéli相Ti6O11透明导电薄膜的厚度为100nm。
接着采用HMS-5300(Ecopia)霍尔效应测试仪对实施例1-4制备得到的Magnéli相Ti6O11透明导电薄膜的电阻率进行检测，采用UV-3600(Shimazu)紫外-可见-红外分光光度计对实施例1-4制备得到的Magnéli相Ti6O11透明导电薄膜的透光光谱进行检测，所有测试都是在大气环境下进行。得到的检测结果图如图1-8所示，数据如下表1所示。
表1
电阻率(Ωcm) 可见光透射率 近红外透射率
实施例1 1.6884x10<sup>-2</sup> 83.58％ 83.68％
实施例2 2.7591x10<sup>-2</sup> 79.74％ 87.42％
实施例3 2.4515x10<sup>-3</sup> 83.68％ 83.43％
实施例4 3.3811x10<sup>-3</sup> 78.18％ 83.98％
由上表可见，制备的Magnéli相Ti6O11透明导电薄膜，具有10-3～10-2量级的电阻率，在可见光有接近或高于80％的透射率，近红外透射率大于80％，可以作为一种新型透明导电薄膜的备选材料。
以上对本发明实施例进行了详细介绍，对于本领域的一般技术人员，依据本发明实施例的思想，在具体实施方式及应用范围上均会有改变之处，综上所述，本说明书内容不应理解为对本发明的限制。

Claims (8)

1.一种高度择优取向Magnéli相Ti6O11透明导电薄膜的制备方法，其特征在于步骤如下：
（1）石英玻璃预处理：将石英玻璃分别在丙酮、无水乙醇、去离子水溶液中超声清洗10min，最后用氮气干燥，备用；
（2）沉积准备：采用脉冲激光沉积法，以石英玻璃作为衬底、TiO2作为靶材，靶材和衬底之间的间距保持在4-8cm，激光束以45°的入射角度照射在靶材表面，先将腔室抽真空为1×10-3-5×10-3 Pa，然后加热衬底温度至200-700℃，再继续抽真空为1×10-4-5×10-4 Pa，接着通氧气，控制氧流量为10sccm，调节氧分压为5-10Pa；
（3）沉积：先预溅射5min，去除靶材表面氧化物后再开始向衬底溅射，结束后原位退火至室温，即生成沉积在石英玻璃衬底上的Magnéli相Ti6O11透明导电薄膜，其中生长速率为2-12 nm/min。
2.根据权利要求1所述的一种高度择优取向Magnéli相Ti6O11透明导电薄膜的制备方法，其特征在于：所述脉冲激光沉积法的设置参数为脉冲激光波长248nm、脉冲宽度25ns、脉冲频率5Hz、输出脉冲能量为200-300 mJ。
3.根据权利要求1所述的一种高度择优取向Magnéli相Ti6O11透明导电薄膜的制备方法，其特征在于：所述TiO2靶材的纯度为99.99%、直径为40 mm、厚度为3 mm。
4.根据权利要求1所述的一种高度择优取向Magnéli相Ti6O11透明导电薄膜的制备方法，其特征在于：所述生成的Magnéli相Ti6O11透明导电薄膜的厚度为30~200nm。
5.一种由权利要求1-4任一项所述的制备方法制备得到的高度择优取向Magnéli相Ti6O11透明导电薄膜。
6.根据权利要求5所述的一种高度择优取向Magnéli相Ti6O11透明导电薄膜，其特征在于：所述透明导电薄膜为纯Magnéli相Ti6O11透明导电薄膜。
7.根据权利要求6所述的一种高度择优取向Magnéli相Ti6O11透明导电薄膜，其特征在于：所述纯Magnéli相Ti6O11透明导电薄膜在(-204)晶面有高度的择优取向性。
8.一种由权利要求1-4任一项所述的制备方法制备得到的高度择优取向Magnéli相Ti6O11透明导电薄膜在宽谱太阳能电池、表面气敏传感器或显示屏中的应用。
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