CN114464691A - 一种GeSn纳米晶材料及其制备方法与应用 - Google Patents

一种GeSn纳米晶材料及其制备方法与应用 Download PDF

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CN114464691A
CN114464691A CN202210119652.1A CN202210119652A CN114464691A CN 114464691 A CN114464691 A CN 114464691A CN 202210119652 A CN202210119652 A CN 202210119652A CN 114464691 A CN114464691 A CN 114464691A
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gesn
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李成
张璐
洪海洋
林光杨
陈松岩
黄巍
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Xiamen University
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Abstract

一种GeSn纳米晶材料及其制备方法与应用，所述GeSn纳米晶材料为GeSn纳米晶嵌于非晶GeSn中，Sn组分的摩尔含量为7.5％～41.6％；所述GeSn纳米晶材料的制备方法，包括以下步骤：1)对衬底进行清洗；2)在清洗后的衬底上，用物理沉积的方法生长局部存在较高Sn组分的非晶GeSn薄膜，以在GeSn薄膜中引入Sn和Ge的浓度梯度；3)对步骤2)的样品进行退火得到非晶GeSn中的高Sn组分GeSn纳米晶。本发明与传统CMOS工艺相兼容，制备得到的GeSn纳米晶的Sn组分高于Sn在Ge中的平衡固溶度并且可通过退火温度调控。

Description

一种GeSn纳米晶材料及其制备方法与应用
技术领域
本发明涉及纳米材料领域，尤其涉及一种GeSn纳米晶材料及其制备方法与应用。
背景技术
纳米材料是指在空间维度上具有纳米尺度的材料，如纳米薄膜、纳米线，纳米带、纳米管及纳米颗粒等。在纳米材料中，由于表面及量子限制等效应的增强，使其具有相比块体材料更加丰富的物理特性。因此，纳米材料不仅是进行基础物理研究的一个优异的平台，还可能用于提高器件的性能或用于新型器件的开发。
GeSn纳米晶作为一类重要的纳米材料，在纳米器件方面具有广阔的应用前景。当GeSn合金中的Sn组分高于6％～10％时，GeSn合金为直接带隙，可用于Si基光电集成芯片的光源。而GeSn纳米晶由于具有量子限制效应，理论上不仅可以通过尺寸调节其发光波长，还能减少材料的自由载流子吸收等光损耗，有望进一步提高GeSn合金的发光性能。截至目前，大部分的GeSn纳米晶是由胶体法制备得到的。然而，胶体法工艺与CMOS工艺不兼容，并且难以将胶体中的量子点均匀的转移到衬底上加以应用。
发明内容
本发明的目的在于解决现有技术中的上述问题，提供一种与CMOS工艺兼容、Sn组分可控的高Sn组分GeSn纳米晶的制备方法，并且制备得到的GeSn纳米晶嵌于非晶GeSn中。
为达到上述目的，本发明采用如下技术方案：
一种GeSn纳米晶材料，GeSn纳米晶嵌于非晶GeSn中，Sn组分的摩尔含量为7.5％～41.6％。
本发明所述一种GeSn纳米晶材料的制备方法，包括以下步骤：
1)对衬底进行清洗；
2)在清洗后的衬底上，用物理沉积的方法生长局部存在较高Sn组分的非晶GeSn薄膜，以在GeSn薄膜中引入Sn和Ge的浓度梯度；
3)对步骤2)的样品进行退火得到非晶GeSn中的高Sn组分GeSn纳米晶。
步骤1)中，所述的衬底包括Si、SOI、SiO2、Ge、GOI衬底。
步骤2)中，所述的非晶GeSn薄膜包括低Sn组分和高Sn组分的GeSn叠层薄膜，GeSn和Sn叠层薄膜，或者Ge和GeSn叠层薄膜。
步骤2)中，所述物理沉积的方法包括溅射、蒸发或分子束外延。
步骤3)中，退火的温度为250～450℃，退火的时间为0.5～40h。
本发明所述GeSn纳米晶材料的应用，用于制备Si基光电子器件。
相对于现有技术，本发明技术方案取得的有益效果是：
本发明与传统CMOS工艺相兼容，制备得到的GeSn纳米晶的Sn组分高于Sn在Ge中的平衡固溶度并且可通过退火温度调控。而且，GeSn纳米晶嵌于非晶中自发形成的结构特点有利于将载流子更好地限制在GeSn纳米晶中，可以用于制作Si基光电子器件。
本发明采用氧化硅作为衬底，利用物理沉积方法进行材料的生长，材料制备成本低，技术成熟。另一方面，通过常规退火方式即能快速简单地获得高Sn组分的GeSn纳米晶并且分散地嵌于非晶中。本发明是一种简易、低成本、与传统CMOS工艺相兼容的制备Sn组分可控的GeSn纳米晶的新方法。
附图说明
图1为实施例1制备的GeSn纳米晶材料的Raman光谱图；
图2为实施例1制备的GeSn纳米晶材料的TEM和电子衍射图。
具体实施方式
为了使本发明所要解决的技术问题、技术方案及有益效果更加清楚、明白，以下结合附图和实施例，对本发明做进一步详细说明。
本发明提供一种与CMOS工艺兼容、Sn组分可控的高Sn组分GeSn纳米晶的制备方法，并且制备得到的GeSn纳米晶嵌于非晶GeSn中，制备方法包括以下步骤：
1)对衬底进行清洗；所述的衬底包括Si、SOI、SiO2、Ge、GOI衬底；
2)在清洗后的衬底上，用物理沉积的方法生长局部存在较高Sn组分的非晶GeSn薄膜，以在GeSn薄膜中引入Sn和Ge的浓度梯度；所述的非晶GeSn薄膜包括低Sn组分和高Sn组分的GeSn叠层薄膜，GeSn和Sn叠层薄膜，或者Ge和GeSn叠层薄膜等组合方式；所述物理沉积的方法包括溅射、蒸发或分子束外延等；
3)对步骤2)的样品利用退火炉进行退火得到嵌于非晶GeSn中的高Sn组分GeSn纳米晶；退火的温度为250～450℃，退火的时间为0.5～40h。
实施例1
本实施例所述GeSn纳米晶材料的制备方法包括以下步骤：
1)对SiO2衬底进行清洗，步骤如下：先将顶层厚度为300nm的SiO2衬底浸泡于丙酮溶液中，放置于超声波清洗机中清洗10min后再将样品浸泡于无水乙醇中，同样放置于超声波清洗机中清洗10min，如此循环3次后用去离子水反复冲洗衬底10次，最后用匀胶机对衬底进行甩干备用。
2)利用溅射制备Ge/Ge0.86Sn0.14薄膜叠层结构。将清洗干净的衬底放入磁控溅射设备中，溅射生长非晶GeSn薄膜以及非晶Ge薄膜堆叠结构，循环10次。其中，非晶GeSn薄膜由Ge和Sn共溅射工艺制备得到，Ge和Sn靶材的纯度分别为99.999％和99.99％。Ge靶利用射频电源进行溅射，功率为100W，Sn靶利用直流电源进行溅射，功率为8.6W。溅射的气氛为Ar，气压为0.5Pa，衬底温度为室温。每层Ge薄膜的厚度均为10nm。GeSn薄膜中的Sn组分为14％，厚度为30nm。
3)利用管式退火炉退火制备GeSn纳米晶。Ge/Ge0.86Sn0.14薄膜叠层结构生长完成后，取出样品并放置于管式退火炉中在N2氛围中进行退火，退火温度设定为385℃，退火时间为40h。
图1为GeSn纳米晶材料的Raman光谱图，其中，Fit Peak 1和Fit Peak 2为非晶Ge-Ge峰，Fit Peak 3为结晶Ge-Ge峰。
图2为GeSn纳米晶材料的TEM和电子衍射图。图2(a)为低分辨样品截面形貌图，上两层结构为Si上SiO2衬底，Ge/GeSn叠层为灰度较深的区域，最下方为TEM制样引入的胶。图2(b,c)为Ge/GeSn叠层的高分辨TEM图，从图中可以看出经过退火后多周期Ge/GeSn叠层演变为均匀的单层薄膜，并且晶粒分布随机，图中白色虚线圈出纳米晶粒，晶粒尺寸范围介于5～15nm。通过图2(d)中的电子衍射图估算GeSn纳米晶材料的Sn组分约为18％。通过控制退火温度可以实现GeSn纳米晶材料的Sn摩尔含量在7.5％～41.6％范围内变化，退火温度越高Sn摩尔含量越低。
本发明的原理如下：
1、步骤2)中局部高Sn组分区域的制备是为了在GeSn薄膜中引入Sn和Ge的浓度梯度。
2、由于GeSn薄膜中存在Sn和Ge组分的局部不均匀，在步骤3)的退火过程中，Sn或Ge首先在浓度梯度的驱动下，通过扩散使其元素均匀分布，由于Sn在Ge中低的固溶度，在低温退火过程中，Sn有偏析的倾向，在薄膜中随机形成多点富集，诱导该区域GeSn晶化，形成高于平均Sn组分的GeSn晶粒。之后，GeSn晶粒逐渐长大，形成嵌于非晶中的高Sn组分GeSn纳米晶，Sn的组分主要取决于退火的温度。

Claims (7)

1.一种GeSn纳米晶材料，其特征在于：GeSn纳米晶嵌于非晶GeSn中，Sn组分的摩尔含量为7.5％～41.6％。
2.权利要求1所述的一种GeSn纳米晶材料的制备方法，其特征在于包括以下步骤：
1)对衬底进行清洗；
2)在清洗后的衬底上，用物理沉积的方法生长局部存在较高Sn组分的非晶GeSn薄膜，以在GeSn薄膜中引入Sn和Ge的浓度梯度；
3)对步骤2)的样品进行退火得到非晶GeSn中的高Sn组分GeSn纳米晶。
3.如权利要求2所述的制备方法，其特征在于：步骤1)中，所述的衬底包括Si、SOI、SiO2、Ge、GOI衬底。
4.如权利要求2所述的制备方法，其特征在于：步骤2)中，所述的非晶GeSn薄膜包括低Sn组分和高Sn组分的GeSn叠层薄膜，GeSn和Sn叠层薄膜，或者Ge和GeSn叠层薄膜。
5.如权利要求2所述的制备方法，其特征在于：步骤2)中，所述物理沉积的方法包括溅射、蒸发或分子束外延。
6.如权利要求2所述的制备方法，其特征在于：步骤3)中，退火的温度为250～450℃，退火的时间为0.5～40h。
7.权利要求1所述的一种GeSn纳米晶材料以及权利要求2～6所述制备方法所制备的GeSn纳米晶材料的应用，其特征在于：用于制备Si基光电子器件。
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