CN106011785A - 一种原子层沉积制备高均匀性Nb掺杂TiO2透明导电薄膜的方法 - Google Patents

一种原子层沉积制备高均匀性Nb掺杂TiO2透明导电薄膜的方法 Download PDF

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CN106011785A
CN106011785A CN201610398336.7A CN201610398336A CN106011785A CN 106011785 A CN106011785 A CN 106011785A CN 201610398336 A CN201610398336 A CN 201610398336A CN 106011785 A CN106011785 A CN 106011785A
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何丹农
卢静
张彦鹏
尹桂林
葛美英
金彩虹
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Shanghai National Engineering Research Center for Nanotechnology Co Ltd
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Abstract

本发明涉及半导体光电材料技术领域的一种原子层沉积制备高均匀性Nb掺杂TiO2透明导电薄膜的方法，通过将超声清洗后氮气吹干的基片加热，采用四氯化钛、三（乙基甲基氨基）叔丁酰胺铌及高纯水作为前驱体源，将沉积组合进行多次循环后制备高均匀性Nb掺杂TiO2透明导电薄膜。该发明制备得到的透明导电薄膜性能优异，折射率在2.3以上，电阻率最低可达2.9×10‑4Ω·cm，此时透光率仍在85%以上。

Description

一种原子层沉积制备高均匀性Nb掺杂TiO2透明导电薄膜的方法
技术领域
本发明属于半导体光电材料制备领域，具体涉及金属Nb掺杂TiO2透明导电薄膜的原子层沉积制备方法。通过原子层复合沉积，能够精确控制金属铌的掺杂均匀性并控制掺杂含量和薄膜膜厚度，获得光电性能明显提高的TiO2基透明导电薄膜。
背景技术
透明导电薄膜（Transparent conducting films）因兼具良好的光学特性与电学特性，在半导体产业中具有广泛的应用，如液晶显示屏、微电子机械系统、太阳能电池及发光二极管等。在过往研究中，铟掺杂氧化锡(ITO)和铝掺杂氧化锌（ZAO）已经获得广泛的应用。但上述材料仍存在较多局限:如铟元素是地球上的稀缺元素并具有一定毒性，折射率有限（均小于2）、在还原气体氛围中不够稳定等。与之相比，二氧化钛具有极高的折射率（2.2-2.4，与硅膜相近）；和机械强度，稳定的化学特性，高的介电常数等优异性能，在半导体光电器件中具有广泛的应用价值，近年来被着重研究过。因而二氧化钛的透明导电薄膜近年来收到广泛的关注。
Nb掺杂TiO2是二氧化钛基透明导电材料中最受关注的一种，研究人员已通过电子束沉积（Thin Solid Films, 525(15) 28–34，2012），溶胶凝胶（Ceramics International, 39(5)，4771–4776）及水热法（Journal of Materials Chemistry A, 3(45)，2015），磁控溅射（蚌埠玻璃工业设计研究院，专利号：201210469093.3）制备Nb掺杂TiO2薄膜，取得一系列进展，但仍存在如下问题：Nb的掺杂含量的难以精确控制、薄膜均匀性及厚度精度等。
2014年，Janne-Petteri Niemel a（Thin Solid Films 551, 19–22,2014)用原子层沉积技术制备Nb掺杂TiO2。在制备过程中采用五乙醇铌[Nb(OEt)5]作为Nb的前驱体源，（需加热至140℃时方能保证完全气化），且制备出的Nb掺杂TiO2薄膜需要经过额外的高温退火才能接近10-4Ω·cm数量级。
发明内容
为克服现有技术的不足，本发明提供一种高质量原子层沉积制备高均匀Nb掺杂TiO2透明导电薄膜的方法。透明导电薄膜的制备方法采用原子层沉积技术，利用三（乙基甲基氨基）叔丁酰胺铌为铌前驱体源，（仅需加热至55℃），通过自限制吸附循环反应过程制备出高均匀度的透明导电二氧化钛掺铌薄膜，通过改变复合循环组合方式精确控制铌的掺杂量与薄膜厚度，使得制备的透明导电薄膜在电阻率低至10-4Ω·cm时，可见光范围内的透光率仍维持在85%以上；这在高精度半导体光电器件上具有广泛的应用价值。
一种原子层沉积制备高均匀性Nb掺杂TiO2透明导电薄膜的方法，其特征在于，
采用四氯化钛为钛前驱体源，三（乙基甲基氨基）叔丁酰胺铌为铌前驱体源，高纯水为氧前驱体源，将基片加热后，采用将前驱体源进行沉积组合进行多组循环后制备出需要的透明导电薄膜；包括如下步骤：
（1）四氯化钛和水在室温下即可，三（乙基甲基氨基）叔丁酰胺铌需加热至55℃；
（2）所采用的沉积组合由n个TiO2沉，n<50，掺杂1个Nb掺杂沉积组成；即进行n个TiO2沉积组合后，引入1个Nb掺杂沉积；
（3）所进行的TiO2沉积是：当沉积腔真空度在15hPa以下时，向沉积腔体引入1个四氯化钛脉冲，后采用高纯氮气清洗沉积腔；后引入1个水蒸汽脉冲进行反应形成单个TiO2原子层与反应残留物，然后用高纯氮气清洗沉积腔；该过程中，四氯化钛脉冲的持续时间为0.4s；氮气清洗时间6s；水蒸气脉冲持续时间为0.2s；氮气冲洗时间4s；将该过程重复n次即可；
（4）所进行的Nb掺杂沉积是：当n个TiO2沉积完成后；引入1个四氯化钛脉冲，持续0.4s，用氮气清洗6s；后引入1个三（乙基甲基氨基）叔丁酰胺铌脉冲；用高纯氮气清洗沉腔后，再引入1个水蒸气脉冲进行反应；接着用高纯氮气清洗沉积腔，完成Nb掺杂沉积；该过程中，三（乙基甲基氨基）叔丁酰胺铌脉冲的持续时间为0.6s，氮气清洗时间8s，水蒸气脉冲持续时间为0.2s，氮气冲洗时间4s。
基片需加热的温度范围应该200-280℃。
本发明的目的是通过以下技术方案来实现的:一种高均匀Nb掺杂TiO2透明导电薄膜的制备方法，制备获得透明导电薄膜均匀性好，电阻率能够低至10-4Ω·cm，可见光范围内的透光率维持在85%以上。具体实现过程为：
（1）采用四氯化钛为钛前驱体源，三（乙基甲基氨基）叔丁酰胺铌为铌前驱体源，高纯水为氧前驱体源。
（2）将超声清洗后氮气枪吹干的玻璃基片加热至一定能够温度后，采用1）中所述的前躯体源进行复合沉积组合的方式进行沉积；其中四氯化钛和水在室温即可；三（乙基甲基氨基）叔丁酰胺铌加热至55℃。
（3）所采用的沉积组合由n个TiO2沉（n<50）掺杂1个Nb掺杂沉积组成；即进行n个TiO2沉积组合后，进行1个Nb掺杂沉积；将该沉积组合进行循环多次。
（4）所进行的TiO2沉积是：当沉积腔真空度在15hPa以下时，向沉积腔体引入四氯化钛，后采用高纯氮气清洗沉积腔；接着引入水蒸汽进行反应形成单个TiO2原子层与反应残留物，再次用高纯氮气清洗沉积腔。该过程中，四氯化钛脉冲的持续时间为0.4s;氮气清洗时间6s;水蒸气脉冲持续时间为0.2s;氮气冲洗时间4s。
（5）所进行的Nb掺杂沉积为：当沉积腔真空度在15Pa以下时，n个TiO2沉积完成后；引入一个四氯化钛脉冲，持续0.4s;用氮气清洗6s；后引入一个三（乙基甲基氨基）叔丁酰胺铌脉冲；用高纯氮气清洗沉腔后，再引入水蒸气进行反应；接着用高纯氮气清洗沉积腔，完成Nb掺杂沉积；该过程中，三（乙基甲基氨基）叔丁酰胺铌脉冲的持续时间为0.6s;氮气清洗时间8s;水蒸气脉冲持续时间为0.2s;氮气冲洗时间4s。
与现有技术，本发明的增益效果是 ：
本发明采用原子层沉积方法，基于TiO2自身的优异的宽禁带性能，采用能够在较低温度下能够气化的三（乙基甲基氨基）叔丁酰胺铌作为铌前驱体源，有效降低了实验条件和能耗；通过先引入四氯化钛，再引入三（乙基甲基氨基）叔丁酰胺铌的掺杂方式，能够有效实现Nb的替位式掺杂，有利于增加载流子浓度提高薄膜的导电性；利用自限制吸附循环反应，直接获得了高均匀性的Nb掺杂TiO2透明导电薄膜。该方法所获得的薄膜电阻率在低至10-4Ω·cm，透光率维持在85%以上。此外原子层沉积工艺过程参数易于控制，通过复合循环设置，能够精确控制Nb的掺杂含量以及制备的薄膜厚度。
附图说明
图1 为实施案例1的可见透射光谱。
具体实施方式
下面对本发明的实施例作详细说明，本实施例在以本发明技术方案为前提下进行实施，给出了详细的实施方式和具体的操作过程，但本发明的保护范围不限于下述的实施例。
实施例1：
将四氯化钛、三（乙基甲基氨基）叔丁酰胺铌及高纯水源装载在机器上，设定三（乙基甲基氨基）叔丁酰胺铌的温度为55℃；当沉积腔加热至200℃后，将采用酒精、丙酮及去离子水超声清洗后的玻璃基片放置沉积腔内；真空抽至15hPa后，进行TiO2循环；即四氯化钛/氮气/水/氮气=（0.4s/6s/0.2s/4s）；循环49次后，进行1次铌掺杂循环，即四氯化钛/氮气/三（乙基甲基氨基）叔丁酰胺铌/氮气/水/氮气=（0.4s/6s/0.6s/8s/0.2s/4s）;该沉积组合为一组循环，将该组循环进行40组；结束后将样品取出，制成厚度约为100nm厚的Nb掺杂TiO2薄膜。经EDS mapping成分，获得Nb的搀杂量约为0.65at.%;此时Nb掺杂TiO2后分子式接近Ti0.98Nb0.02O2;图1
实施例2：
将四氯化钛、三（乙基甲基氨基）叔丁酰胺铌及高纯水源装载在机器上，设定三（乙基甲基氨基）叔丁酰胺铌的温度为55℃；当沉积腔加热至220℃后，将采用酒精、丙酮及去离子水超声清洗后的玻璃基片放置沉积腔内；真空抽至15hPa后，进行TiO2循环；即四氯化钛/氮气/水/氮气=（0.4s/6s/0.2s/4s）；循环24次后，进行1次铌掺杂循环，即四氯化钛/氮气/三（乙基甲基氨基）叔丁酰胺铌/氮气/水/氮气=（0.4s/6s/0.6s/8s/0.2s/4s）;该沉积组合为一组循环，将该组循环进行80组；结束后将样品取出，制成厚度约为100nm厚的Nb掺杂TiO2薄膜。经EDS mapping成分，获得Nb的搀杂量约为1.31at.%; 此时Nb掺杂TiO2后分子式接近Ti0.96Nb0.04O2;
实施例3：
将四氯化钛、三（乙基甲基氨基）叔丁酰胺铌及高纯水源装载在机器上，设定三（乙基甲基氨基）叔丁酰胺铌的温度为55℃；当沉积腔加热至240℃后，将采用酒精、丙酮及去离子水超声清洗后的玻璃基片放置沉积腔内；真空抽至15hPa后，进行TiO2循环；即四氯化钛/氮气/水/氮气=（0.4s/6s/0.2s/4s）；循环19次后，进行1次铌掺杂循环，即四氯化钛/氮气/三（乙基甲基氨基）叔丁酰胺铌/氮气/水/氮气=（0.4s/6s/0.6s/8s/0.2s/4s）;该沉积组合为一组循环，将该组循环进行100组；结束后将样品取出，制成厚度约为100nm厚的Nb掺杂TiO2薄膜。经EDS mapping成分，获得Nb的搀杂量约为1.65at.%; 此时Nb掺杂TiO2后分子式接近Ti0.95Nb0.05O2;
实施案例4：
将四氯化钛、三（乙基甲基氨基）叔丁酰胺铌及高纯水源装载在机器上，设定三（乙基甲基氨基）叔丁酰胺铌的温度为55℃；当沉积腔加热至260℃后，将采用酒精、丙酮及去离子水超声清洗后的玻璃基片放置沉积腔内；真空抽至15hPa后，进行TiO2循环；即四氯化钛/氮气/水/氮气=（0.4s/6s/0.2s/4s）；循环9次后，进行1次铌掺杂循环，即四氯化钛/氮气/三（乙基甲基氨基）叔丁酰胺铌/氮气/水/氮气=（0.4s/6s/0.6s/8s/0.2s/4s）;该沉积组合为一组循环，将该组循环进行200组；结束后将样品取出，制成厚度约为100nm厚的Nb掺杂TiO2薄膜。经EDS mapping成分，获得Nb的搀杂量约为3.31at.%; 此时Nb掺杂TiO2后分子式接近Ti0.9Nb0.1O2;
实施案例5:
将四氯化钛、三（乙基甲基氨基）叔丁酰胺铌及高纯水源装载在机器上，设定三（乙基甲基氨基）叔丁酰胺铌的温度为55℃；当沉积腔加热至280℃后，将采用酒精、丙酮及去离子水超声清洗后的玻璃基片放置沉积腔内；真空抽至15hPa后，进行TiO2循环；即四氯化钛/氮气/水/氮气=（0.4s/6s/0.2s/4s）；循环4次后，进行1次铌掺杂循环，即四氯化钛/氮气/三（乙基甲基氨基）叔丁酰胺铌/氮气/水/氮气=（0.4s/6s/0.6s/8s/0.2s/4s）;该沉积组合为一组循环，将该组循环进行400组；制成厚度约为100nm厚的Nb掺杂TiO2薄膜。经EDS mapping成分，获得Nb的搀杂量约为6.74at.%, 此时Nb掺杂TiO2后分子式接近Ti0.8Nb0.2O2;
对实施案例样品进行光学及电学特性性能测试，测试结果如表格1）所示：
表 1 ：

Claims (2)

1.一种原子层沉积制备高均匀性Nb掺杂TiO2透明导电薄膜的方法，其特征在于，
采用四氯化钛为钛前驱体源，三（乙基甲基氨基）叔丁酰胺铌为铌前驱体源，高纯水为氧前驱体源，将基片加热后，采用将前驱体源进行沉积组合进行多组循环后制备出需要的透明导电薄膜；包括如下步骤：
（1）四氯化钛和水在室温下即可，三（乙基甲基氨基）叔丁酰胺铌需加热至55℃；
（2）所采用的沉积组合由n个TiO2沉，n<50，掺杂1个Nb掺杂沉积组成；即进行n个TiO2沉积组合后，引入1个Nb掺杂沉积；
（3）所进行的TiO2沉积是：当沉积腔真空度在15hPa以下时，向沉积腔体引入1个四氯化钛脉冲，后采用高纯氮气清洗沉积腔；后引入1个水蒸汽脉冲进行反应形成单个TiO2原子层与反应残留物，然后用高纯氮气清洗沉积腔；该过程中，四氯化钛脉冲的持续时间为0.4s；氮气清洗时间6s；水蒸气脉冲持续时间为0.2s；氮气冲洗时间4s；将该过程重复n次即可；
（4）所进行的Nb掺杂沉积是：当n个TiO2沉积完成后；引入1个四氯化钛脉冲，持续0.4s，用氮气清洗6s；后引入1个三（乙基甲基氨基）叔丁酰胺铌脉冲；用高纯氮气清洗沉腔后，再引入1个水蒸气脉冲进行反应；接着用高纯氮气清洗沉积腔，完成Nb掺杂沉积；该过程中，三（乙基甲基氨基）叔丁酰胺铌脉冲的持续时间为0.6s，氮气清洗时间8s，水蒸气脉冲持续时间为0.2s，氮气冲洗时间4s。
2. 根据权利要求1所述原子层沉积制备高均匀性Nb掺杂TiO2透明导电薄膜的方法，其特征在于，基片需加热的温度范围应该200-280℃。
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