CN105483617A - 一种在非硅衬底上制备Mg2Si薄膜的方法 - Google Patents

一种在非硅衬底上制备Mg2Si薄膜的方法 Download PDF

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CN105483617A
CN105483617A CN201511002465.1A CN201511002465A CN105483617A CN 105483617 A CN105483617 A CN 105483617A CN 201511002465 A CN201511002465 A CN 201511002465A CN 105483617 A CN105483617 A CN 105483617A
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谢泉
廖杨芳
肖清泉
梁枫
王善兰
吴宏仙
房迪
张晋敏
陈茜
谢晶
范梦慧
黄晋
章竞予
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Abstract

本发明公开了一种在非硅衬底上制备Mg2Si薄膜的方法，其特征在于：包含以下步骤：第一、在清洁的非硅衬底上沉积一层Si膜，然后在Si膜上沉积一层Mg膜；第二、退火工艺，沉积完成后的样品置于高真空退火炉中进行低真空氛围退火，最后制备得到Mg2Si半导体薄膜。

Description

一种在非硅衬底上制备Mg2Si薄膜的方法
技术领域
本发明涉及一种Mg2Si半导体薄膜的制备方法，尤其涉及一种在非硅衬底上制备Mg2Si半导体薄膜的方法。
背景技术
Mg2Si是一种具有反萤石结构的金属硅化物环境友好半导体材料，价格低廉、元素无毒无污染。带隙值在0.6eV-0.8eV之间，在红外传感器、红外光LED等光电器件领域具有广阔的应用前景；具有很高的热电系数(ZT>1)、很低的热导率和电阻率，在热电器件中具有重要应用价值。它有望逐步取代以前有毒或容易造成环境污染的半导体材料，具有较大的社会效益及环境效益。目前，国内外Mg2Si薄膜主要是在硅衬底上制备的，如利用磁控溅射、热蒸发、热扩散方法在硅衬底上沉积一层Mg经高温退火后形成Mg2Si薄膜(专利CN201010147304.2，CN201210455881.7，CN200710064777.4)，或采用分子束外延技术镁硅共沉积的方法在硅衬底上制备出Mg2Si薄膜（文献PHYSICALREVIEWB，VOLUME54,NUMBER23）。这些方法虽然均能制备出高质量的Mg2Si薄膜，但由于以下几个方面的原因，这些方法在Mg2Si薄膜器件制备中受到很大的限制。（1）硅衬底的导电类型会直接影响Mg2Si薄膜导电类型的测试，如硅衬底为n型，测得的未刻意掺杂的Mg2Si薄膜也为n型；若硅衬底为p型，测得的未刻意掺杂的Mg2Si薄膜也为p型。因此在硅衬底上无法直接获得Mg2Si薄膜的导电类型。（2）由于在硅衬底上生长的Mg2Si薄膜是利用金属镁的高活性，在适当的温度下与硅进行固相反应而得到的。反应后，Mg2Si与硅的界面很不平整，存在诸多缺陷，这些缺陷将会严重影响Mg2Si薄膜器件的性质。（3）由于硅的导热性能很好，而具有良好性能的热电器件的关键因素是材料的热导率尽可能低，所以在硅衬底上制备Mg2Si薄膜热电器件受到了极大的限制。（4）LED产业中，蓝宝石衬底是目前的主流选择，几乎占据99%的市场，其制造技术成熟性、稳定性等方面现在都比硅衬底好，硅衬底LED的良率、光效以及成本等依旧是当下亟待解决的问题，因此，其市场认同度不够，参与推广应用的企业少。
发明内容
本发明要解决的技术问题是：供一种在非硅衬底上制备高质量的Mg2Si半导体薄膜的方法，以克服现有技术存在的硅衬底上的Mg2Si薄膜导电类型无法直接测量、Mg2Si/Si界面缺陷密度大、硅衬底上的热电器件性能不佳、硅衬底LED的良率低、光效差、难于工业化推广等缺点。
本发明的技术方案是：一种在非硅衬底上制备Mg2Si薄膜的方法，包含以下步骤：第一、在清洁的非硅衬底上沉积一层Si膜,然后在Si膜上沉积一层Mg膜；第二、退火工艺，沉积完成后的样品置于高真空退火炉中进行低真空氛围退火，最后制备得到Mg2Si半导体薄膜。
所述非硅衬底为玻璃衬底、石英衬底、蓝宝石衬底、GaN衬底、GaAs衬底、SiC衬底或石墨衬底。
所述高真空薄膜沉积系统为磁控溅射系统、热蒸发系统薄膜的物理气相沉积系统。
Si膜厚度为125-225nm。
Mg膜的厚度为190-250nm。
在沉积Si膜和Mg膜前，对预先装在真空系统的Si和Mg预处理，以去除Si、Mg表面的氧化物污染物。
退火前对退火炉抽真空，使其背底真空小于等于10-4Pa。
退火过程中，保持退火炉腔体内气压为10-1-10-2Pa，退火时间为3.5-4.5小时，退火温度为350-450℃。
本发明的有益效果：由于采用了上述技术方案，与现有技术相比，本发明在非硅衬底上成功制备了结晶质量好、表面平整的Mg2Si半导体薄膜，合成的Mg2Si薄膜中不含富余的Mg或Si，也不含MgO或SiO2等杂质，为Mg2Si半导体薄膜的器件开发利用奠定良好的基础。本发明制备的Mg2Si薄膜的导电类型不受衬底影响；能与其它半导体材料形成界面平整、缺陷密度低的高质量异质结；能充分利用Mg2Si是优良的热电材料这一性质制备出高质量的热电器件；能大大提高基于Mg2Si薄膜的LED的效率。本发明利用的磁控溅射或热蒸发设备简单、易于操作，可以制备均匀、大面积的薄膜，有利于工业化大规模生产。
附图说明
图1为本发明在非硅衬底上制备Mg2Si薄膜的工艺流程图；
图2为本发明的样品X射线衍射图，在玻璃衬底上先溅射25minN-Si，再溅射15minMg然后退火形成的Mg2Si薄膜的X射线衍射图；
图3为本发明的样品X射线衍射图，在玻璃衬底上先溅射25minN-Si，再溅射17.5minMg然后退火形成的Mg2Si薄膜的X射线衍射图；
图4为本发明的样品X射线衍射图，在玻璃衬底上先溅射25minN-Si，再溅射20minMg然后退火形成的Mg2Si薄膜的X射线衍射图；
图5为本发明的样品扫描电镜图，在玻璃衬底上先溅射25minN-Si，再溅射15minMg然后退火形成的Mg2Si薄膜的扫描电镜图；
图6为本发明的样品扫描电镜图，在玻璃衬底上先溅射25minN-Si，再溅射17.5minMg然后退火形成的Mg2Si薄膜的扫描电镜图；
图7为本发明的样品扫描电镜图，在玻璃衬底上先溅射25minN-Si，再溅射20minMg然后退火形成的Mg2Si薄膜的扫描电镜图。
具体实施方式
本发明的实施例：
（1）清洗玻璃基片。玻璃基片分别用双氧水、丙酮、乙醇、去离子水超声清洗20分钟，吹干后送入磁控溅射系统的样品室，进行反溅射清洁玻璃基片表面。之后送入磁控溅射系统的溅射室。
（2）在玻璃基片上直流溅射沉积Si膜。溅射室背底气压为2.0x10-5Pa。溅射沉积过程中，溅射功率为110W，氩气(99.999%纯度)流量15sccm，溅射气压为2.0Pa，溅射时间为25min，这样的沉积条件下，溅射沉积Si膜的厚度约175nm。溅射时衬底温度为室温。在溅射Si膜前，首先对预先装在溅射室的Si靶预溅射，去除Si靶上的氧化物。
（3）在Si膜上射频溅射沉积Mg膜。溅射沉积过程中，溅射功率为100W，氩气(99.999%纯度)流量30sccm，溅射气压为3.0Pa，溅射时间为15-20min，这样的沉积条件下，溅射沉积Mg膜的厚度约190-250nm。溅射时衬底温度为室温。在溅射Mg膜前，首先对预先装在溅射室的Mg靶预溅射，去除Mg靶上的氧化物。
（4）将衬底/Si/Mg样品放入高真空退火炉中退火。退火炉背底气压为4.0x10- 4Pa。退火时气压保持在1.5x10-2Pa，退火时间为4h，退火温度为400℃。
上述薄膜制备完成后，我们利用X射线衍射仪和扫描电镜对薄膜进行了测试，结果表明：
从图2-4中所示相同的Si膜厚度、不同的Mg膜厚度的X射线衍射图可以看出，生成的Mg2Si结晶质量非常好，具有高度的（220）择优取向。
从图5-7中所示的相同的Si膜厚度、不同的Mg膜厚度的扫描电镜图（放大10000倍）可以看出，生成的Mg2Si晶粒分布均匀，表面非常平整，说明制备的Mg2Si薄膜质量很好。
以上所述仅为本发明的较佳实例而已，并非用于限定本发明的保护范围，凡在本发明的精神和原则之内所做的任何修改等同替换以及改进，均应包含在本发明的保护范围之内。

Claims (8)

1.一种在非硅衬底上制备Mg2Si薄膜的方法，其特征在于：包含以下步骤：第一、在清洁的非硅衬底上沉积一层Si膜,然后在Si膜上沉积一层Mg膜；第二、退火工艺，沉积完成后的样品置于高真空退火炉中进行低真空氛围退火，最后制备得到Mg2Si半导体薄膜。
2.根据权利要求1所述的一种在非硅衬底上制备Mg2Si薄膜的方法，其特征在于：所述非硅衬底为玻璃衬底、石英衬底、蓝宝石衬底、GaN衬底、GaAs衬底、SiC衬底或石墨衬底。
3.根据权利要求1所述的一种在非硅衬底上制备Mg2Si薄膜的方法，其特征在于：所述高真空薄膜沉积系统为磁控溅射系统、热蒸发系统薄膜的物理气相沉积系统。
4.根据权利要求1所述的一种在非硅衬底上制备Mg2Si薄膜的方法，其特征在于：Si膜厚度为125-225nm。
5.根据权利要求1所述的一种在非硅衬底上制备Mg2Si薄膜的方法，其特征在于：Mg膜的厚度为190-250nm。
6.根据权利要求1所述的一种在非硅衬底上制备Mg2Si薄膜的方法，其特征在于：在沉积Si膜和Mg膜前，对预先装在真空系统的Si和Mg预处理，以去除Si、Mg表面的氧化物污染物。
7.根据权利要求1所述的一种在非硅衬底上制备Mg2Si薄膜的方法，其特征在于：退火前对退火炉抽真空，使其背底真空小于等于10-4Pa。
8.根据权利要求1所述的一种在非硅衬底上制备Mg2Si薄膜的方法，其特征在于：退火过程中，保持退火炉腔体内气压为10-1-10-2Pa，退火时间为3.5-4.5小时，退火温度为350-450℃。
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