CN106637204A - Ag/ZnO/Mg光电透明导电薄膜的沉积方法 - Google Patents

Ag/ZnO/Mg光电透明导电薄膜的沉积方法 Download PDF

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CN106637204A
CN106637204A CN201611094524.7A CN201611094524A CN106637204A CN 106637204 A CN106637204 A CN 106637204A CN 201611094524 A CN201611094524 A CN 201611094524A CN 106637204 A CN106637204 A CN 106637204A
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梁结平
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Abstract

本发明涉及一种Ag/ZnO/Mg光电透明导电薄膜的沉积方法，属透明导电材料领域。本发明一种按照以下步骤进行：(1)将基片用丙酮、乙醇以及去离子水用超声波依次清洗后，用氮气吹干送入反应室；2)磁控溅射Mg膜的沉积；(3)有机物化学气相沉积制备中间层ZnO薄膜：(4)磁控溅射Ag膜的沉积：(5)对Ag/ZnO/Mg的多层结构的透明导电薄膜进行高温退火，退火温度为200～600℃，退火时间为20min，得到Ag、Mg共同掺杂的ZnO光电透明导电薄膜。本发明制备工艺简单，沉积过程易于控制。本发明制备的透明导电薄膜均匀性好，光电性能优异，电阻率可低至7.0×10‑4Ω·cm，而其透光率可达85％以上。可用于制造太阳能电池、发光二极管、LCD以及手机等光电器件的透明电极。

Description

Ag/ZnO/Mg光电透明导电薄膜的沉积方法
技术领域
本发明属透明导电材料领域，特别涉及一种Ag/ZnO/Mg光电透明导电薄膜的沉积方法。
背景技术
随着社会发展和科学技术的突飞猛进，人类对功能材料的需求日益增加，新型功能材料已成为新技术和新兴工业发展的关键。随着太阳能、平板显示和半导体照明等产业的发展，一种新的功能材料——透明导电材料随之产生、发展起来。
透明导电膜玻璃即透明导电氧化物镀膜玻璃，是在平板玻璃表面通过物理或者化学镀膜的方法均匀镀上一层TCO薄膜。目前应用中的TCO材料主要为三类，ITO-In2O3基薄膜(Sn掺杂)、FTO-SnO2基薄膜(F掺杂)和AZO-ZnO基薄膜(Al掺杂)等。
ITO-In2O3的晶体结构为体心立方铁锰矿结构，禁带宽度约3.5eV，因而在可见光范围透明，Tavg〉90％。ITO最低电阻率可达10-5Ω.cm量级。ITO是目前最成熟、应用最广泛的TCO，目前除了TFT-LCD面板几乎都使用ITO外，替代传统的太阳能电池的铝背电极而形成新型的太阳能电池的透明导电电极和薄膜太阳能电池也都使用。不过由于ITO须使用稀有金属铟(中国铟保有储量1.3万吨，约占全球2/3)，从而导致生产成本很高。随着TFT-LCD面板市场持续扩增和太阳能电池的进一步发展，全球铟消费量的83％用于ITO，从而也引发了铟矿在未来将逐渐耗尽的问题。而且铟材料有毒，在制备和应用过程中对人体有害。另外铟和锡的原子量较大，成膜过程中容易渗入到衬底内部，毒化衬底材料，尤其在液晶显示器件中污染现象严重。对于太阳能行业来说，TCO玻璃必须具备提高光散射的能力，而ITO镀膜很难做到这一点，并且激光刻蚀性能较差、ITO在等离子体中并不够稳定(一般硅薄膜太阳能电池需要在等离子体条件下制作)，因此目前ITO已非光伏电池主流的电极材料。总之，寻找合适的替代产品势在必行。
FTO-SnO2具有正四面体的金红石结构，禁带宽度为3.6eV，通过掺杂氟得到FTO薄膜，可以进一步增强导电性能。FTO与ITO相比具有热稳定性高、耐腐蚀、硬度高等优势，并且在等离子体中也具有很好的稳定性，从而成为目前商业化应用的光伏TCO材料。但是，高结晶质量FTO薄膜制备比较困难，对制备工艺要求高，由于薄膜内部缺陷的存在而使其透光率与电导率低于ITO薄膜；同时由于需要氟元素(剧毒)掺杂因而工艺过程存在一定的污染。此外，由于FTO薄膜硬度高因而比较难于刻蚀。
ZnO基薄膜。ZnO属于N型Ⅱ－Ⅵ族半导体材料，其晶体结构为六方纤锌矿结构禁带宽度约3.4eV，透光率可达90％以上。同时ZnO在不掺杂的情况下由于本征氧空位缺陷的存在也具有较高的电导率，通过III族元素(Al、Ga、B)掺杂可以进一步提高导电性。ZnO用于TCO薄膜具有原料丰富、成本低廉、制备工艺简单、无毒、不污染环境等显著的优势。而且，ZnO能够在氢等离子体中稳定性要优于ITO薄膜，具有可与ITO薄膜相比拟的光电特性的同时又易于刻蚀。另外ZnO可高效透射ITO难以透射的短波长光线，因而无论是在太阳能电池还是平板显示上，ZnO都是替代ITO与FTO的有力竞争者。
发明内容
针对现有材料存在的不足，本发明通过在基片衬底上依次进行磁控溅射Mg薄膜，然后利用有机物化学气相沉积制备中间层ZnO薄膜，最后磁控溅射Ag薄膜，之后对实验薄膜样品进行高温退火处理，得到Ag/ZnO/Mg结构的透明导电薄膜。
本发明一种Ag/ZnO/Mg光电透明导电薄膜的沉积方法，其特征在于按照以下步骤进行：
(1)将基片用丙酮、乙醇以及去离子水用超声波依次清洗后，用氮气吹干送入反应室；
(2)磁控溅射Mg膜的沉积：将沉积室本底抽到9.5×10-4Pa之后，通入氩气，在基片衬底上射频溅射Mg靶材，沉积制备厚度为20～60nmMg薄膜；
(3)有机物化学气相沉积制备中间层ZnO薄膜：将沉积反应室真空抽至7.5×10-4Pa后，将沉积上Mg膜的基片加热至50～450℃，向反应室内同时通入氩气携带的Zn(CH2CH3)2和O2，Zn(CH2CH3)2和O2量由质量流量计控制流量比为(2～4)：(200～400)，控制气体总压强为0.9～2.1Pa；在电子回旋共振频率为750W，反应25～45min,得到450～650nm的ZnO薄膜；
(4)磁控溅射Ag膜的沉积：将沉积室本底抽到8.5×10-4Pa之后，通入氩气，在ZnO/Mg基片上射频溅射Ag靶材，沉积制备厚度为15～45nm的Ag薄膜；
(5)对Ag/ZnO/Mg的多层结构的透明导电薄膜进行高温退火，退火温度为200～600℃，退火时间为20min，得到Ag、Mg共同掺杂的ZnO光电透明导电薄膜。
作为优选，所述基片为普通康宁玻璃、蓝宝石、石英、太阳能电池片、硅片或有机聚合物。
作为优选，所述步骤(2)中磁控溅射Mg膜的沉积条件具体为：对基片衬底进行加热至150℃并调整氩气气体流量使气压达到6Pa，溅射功率为150W，溅射时间为2～6min，使得Mg薄膜厚度为20～60nm。
作为优选，所述步骤(4)磁控溅射Ag膜的沉积条件具体为：ZnO/Mg基片进行加热至200℃，并调整氩气气体流量使气压达到9Pa，溅射功率为150W，溅射时间为1～4min，使得Ag膜的厚度是15～45nm。
本发明采用等离子增强电子回旋共振有机物化学气相沉积技术与磁控溅射技术相结合的方式，利用ZnO良好的光电性能和Ag、Mg的低电阻率，形成Ag/ZnO/Mg的结构，在经过高温退火处理。由于Ag、Mg的掺入，载流子浓度增加，薄膜的导电性能得到了很大的提高，同时可保持透光率达到85％以上。
本发明制备工艺简单，沉积过程易于控制。本发明制备的透明导电薄膜均匀性好，光电性能优异，电阻率可低至7.0×10-4Ω·cm，而其透光率可达85％以上。可用于制造太阳能电池、发光二极管、LCD以及手机等光电器件的透明电极。
附图说明
图1为本发明方法得到的Ag/ZnO/Mg透明导电薄膜示意图。
图中1为基片，2为Mg薄膜，3为中间层ZnO透明导电薄膜，4为Ag薄膜。
具体实施方式
下面通过实施例对本发明的内容进一步说明，本发明的保护范围不限于下述的实施例。
实施例1
将基片用丙酮、乙醇以及去离子水用超声波依次清洗后，用氮气吹干送入反应室。
将磁控溅射的本底真空抽至9.5×10-4Pa后，对基片衬底进行加热至150℃并调整气体流量使气压达到6Pa，溅射功率为150W，溅射时间为2min，Mg薄膜厚度为20nm。
然后，利用等离子增强电子回旋共振化学气相沉积的方法沉积制备ZnO薄膜，真空抽至7.5×10-4Pa后，将基片加热至150℃，向反应室内同时通入氩气携带的Zn(CH2CH3)2和O2后，Zn(CH2CH3)2和O2量由质量流量计控制流量比为2sccm：200sccm，控制气体总压强为1.5Pa；在电子回旋共振频率为750W，反应25min,得到450nm的ZnO薄膜。
然后将所制备的薄膜经过清洗处理后其放入磁控溅射室，进行Ag薄膜的溅射，对基片衬底进行加热至200℃并调整气体流量使气压达到9Pa，溅射功率为150W，溅射时间为1min的Ag薄膜，其薄膜厚度为15nm。
最后在高温的情形下对该结构薄膜进行高温退火处理，其退火温度为200℃，退火时间为20min。得到的Ag/ZnO/Mg透明导电薄膜示意图如图1所示，1为基片，2为Mg薄膜，3为中间层ZnO透明导电薄膜，4为Ag薄膜。
对Ag/ZnO/Mg光电透明导电薄膜的电学性能进行了测试，其与普通磁控溅射沉积制备ZnO的电学性能对比如表1所示，由表1可以看出Ag/ZnO/Mg光电透明导电薄膜与普通磁控溅射沉积制备ZnO薄膜相比，电阻率明显降低，迁移率和载流子浓度明显增加。
表1 Ag/ZnO/Mg光电透明导电薄膜的沉积方法与普通磁控溅射沉积制备ZnO的电学性能对比
实施例2
将基片用丙酮、乙醇以及去离子水用超声波依次清洗后，用氮气吹干送入反应室。
将磁控溅射的本底真空抽至9.5×10-4Pa后，对基片衬底进行加热至150℃并调整气体流量使气压达到6Pa，溅射功率为150W，溅射时间为6min，Mg薄膜厚度为60nm。
然后，利用等离子增强电子回旋共振化学气相沉积的方法沉积制备ZnO薄膜，真空抽至7.5×10-4Pa后，将基片加热至300℃，向反应室内同时通入氩气携带的Zn(CH2CH3)2和O2后，Zn(CH2CH3)2和O2量由质量流量计控制流量比为4sccm：200sccm，控制气体总压强为1.5Pa；在电子回旋共振频率为750W，反应45min,得到650nm的ZnO薄膜。
然后将所制备的薄膜经过清洗处理后其放入磁控溅射室，进行Ag薄膜的溅射，对基片衬底进行加热至200℃并调整气体流量使气压达到9Pa，溅射功率为150W，溅射时间为4min的Ag薄膜，其薄膜厚度为45nm。
最后在高温的情形下对该结构薄膜进行高温退火处理，其退火温度为600℃，退火时间为20min，以得到的Ag/ZnO/Mg透明导电薄膜，对Ag/ZnO/Mg光电透明导电薄膜的电学性能进行了测试，其与普通磁控溅射沉积制备ZnO的电学性能对比如表2所示，由表2可以看出Ag/ZnO/Mg光电透明导电薄膜与普通磁控溅射沉积制备ZnO薄膜相比，电阻率明显降低，迁移率和载流子浓度明显增加。
表2Ag/ZnO/Mg光电透明导电薄膜的沉积方法与普通磁控溅射沉积制备ZnO的电学性能对比
以上所述是本发明的优选实施方式，应当指出，对于本技术领域的普通技术人员来说，在不脱离本发明原理的前提下，还可以做出若干改进和润饰，这些改进和润饰也视为本发明的保护范围。

Claims (4)

1.一种Ag/ZnO/Mg光电透明导电薄膜的沉积方法，其特征在于按照以下步骤进行：
(1)将基片用丙酮、乙醇以及去离子水用超声波依次清洗后，用氮气吹干送入反应室；
(2)磁控溅射Mg膜的沉积：将沉积室本底抽到9.5×10-4Pa之后，通入氩气，在基片衬底上射频溅射Mg靶材，沉积制备厚度为20～60nmMg薄膜；
(3)有机物化学气相沉积制备中间层ZnO薄膜：将沉积反应室真空抽至7.5×10-4Pa后，将沉积上Mg膜的基片加热至50～450℃，向反应室内同时通入氩气携带的Zn(CH2CH3)2和O2，Zn(CH2CH3)2和O2量由质量流量计控制流量比为(2～4)：(200～400)，控制气体总压强为0.9～2.1Pa；在电子回旋共振频率为750W，反应25～45min,得到450～650nm的ZnO薄膜；
(4)磁控溅射Ag膜的沉积：将沉积室本底抽到8.5×10-4Pa之后，通入氩气，在ZnO/Mg基片上射频溅射Ag靶材，沉积制备厚度为15～45nm的Ag薄膜；
(5)对Ag/ZnO/Mg的多层结构的透明导电薄膜进行高温退火，退火温度为200～600℃，退火时间为20min，得到Ag、Mg共同掺杂的ZnO光电透明导电薄膜。
2.根据权利要求1所述的一种Ag/ZnO/Mg光电透明导电薄膜的沉积方法，其特征在于所述基片为普通康宁玻璃、蓝宝石、石英、太阳能电池片、硅片或有机聚合物。
3.根据权利要求1所述的一种Ag/ZnO/Mg光电透明导电薄膜的沉积方法，其特征在于所述步骤(2)中磁控溅射Mg膜的沉积条件具体为：对基片衬底进行加热至150℃并调整氩气气体流量使气压达到6Pa，溅射功率为150W，溅射时间为2～6min，使得Mg薄膜厚度为20～60nm。
4.根据权利要求1所述的一种Ag/ZnO/Mg光电透明导电薄膜的沉积方法，其特征在于所述步骤(4)磁控溅射Ag膜的沉积条件具体为：ZnO/Mg基片进行加热至200℃，并调整氩气气体流量使气压达到9Pa，溅射功率为150W，溅射时间为1～4min，使得Ag膜的厚度是15～45nm。
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